ICS-2000 ION CHROMATOGRAPHY SYSTEM OPERATOR’S MANUAL
Document No. 031857 Revision 03 April 2006
©2006 by Dionex Corporation All rights reserved worldwide. Printed in the United States of America. This publication is protected by federal copyright law. No part of this publication may be copied or distributed, transmitted, transcribed, stored in a retrieval system, or transmitted into any human or computer language, in any form or by any means, electronic, mechanical, magnetic, manual, or otherwise, or disclosed to third parties without the express written permission of Dionex Corporation, 1228 Titan Way, Sunnyvale, California 94088-3603 U.S.A.
DISCLAIMER OF WARRANTY AND LIMITED WARRANTY THIS PUBLICATION IS PROVIDED “AS IS” WITHOUT WARRANTY OF ANY KIND. DIONEX CORPORATION DOES NOT WARRANT, GUARANTEE, OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE, OR THE RESULTS OF THE USE, OF THIS PUBLICATION IN TERMS OF CORRECTNESS, ACCURACY, RELIABILITY, CURRENTNESS, OR OTHERWISE. FURTHER, DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES.
TRADEMARKS AES, Atlas, Chromeleon, EluGen, IonPac, OnGuard, and SRS are registered trademarks of Dionex Corporation. CarboPac, MicroMembrane, MMS, ReagentFree, and RFIC are trademarks of Dionex Corporation. Acrobat, Adobe, and Adobe Reader, are registered trademarks of Adobe Systems, Incorporated. PEEK is a trademark of Victrex PLC. Teflon is a registered trademark of E.I. duPont de Nemours & Company. Microsoft and Windows are registered trademarks of Microsoft Corporation.
PRINTING HISTORY Revision 01, March 2003 Revision 02, September 2005 Revision 03, March 2006
Contents
1 • Introduction 1.1
Introduction to Ion Chromatography (IC) . . . . . . . . . . . . . . . . . . . . . . .1-1
1.2
Overview of the ICS-2000 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4
1.3
About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-5 1.3.1
Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . .1-6
1.3.2
Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-8
2 • Features 2.1
2.2
Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1 2.1.1
Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1
2.1.2
Top Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-6
2.1.3
Component Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7
2.1.4
Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-10
The Chromeleon Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-12 2.2.1
The Chromeleon Main Window and Browser . . . . . . . . . . . .2-12
2.2.2
The ICS-2000 Control Panels . . . . . . . . . . . . . . . . . . . . . . . . .2-13
2.3
Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-23
2.4
System Component Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-30
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2.4.1
Vacuum Degas Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . .2-30
2.4.2
Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-32
2.4.3
Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-32
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ICS-2000 Ion Chromatography System
2.4.4
Eluent Generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-35
2.4.5
Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-40
2.4.6
Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-42
2.4.7
Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-42
2.4.8
DS6 Heated Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . 2-43
3 • Operation and Maintenance 3.1
Operation Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
3.2
Power Up the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
3.3
Start Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
3.4
Set Up the Eluent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6 Filter the Deionized Water . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
3.4.2
Fill the Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
3.4.3
Set the Eluent Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7
3.4.4
Connect the Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
3.5
Check All Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
3.6
Prime the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10
3.7
Set System Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11
3.8
Equilibrate the System and Verify Operational Status . . . . . . . . . . . 3-12
3.9
Prepare Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
3.10
ii
3.4.1
3.9.1
Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . . 3-13
3.9.2
Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
3.9.3
Diluting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Loading and Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
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Contents
3.10.1 Loading Samples with a Syringe . . . . . . . . . . . . . . . . . . . . . .3-15 3.10.2 Loading Samples with a Vacuum Syringe . . . . . . . . . . . . . . .3-16 3.10.3 Loading Samples with an Autosampler . . . . . . . . . . . . . . . . .3-16 3.10.4 Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-17 3.10.5 Example Chromeleon Commands for Loading and Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-17 3.11
Process Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-18 3.11.1 Manual Sample Processing . . . . . . . . . . . . . . . . . . . . . . . . . .3-18 3.11.2 Automatic (Batch) Sample Processing . . . . . . . . . . . . . . . . . .3-19
3.12
Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-21
4 • Troubleshooting 4.3
Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1
4.1
Troubleshooting Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-3
4.2
Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-12
4.3
Pump Difficult to Prime or Loses Prime . . . . . . . . . . . . . . . . . . . . . . .4-14
4.4
Pump Does Not Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-16
4.5
No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-17
4.6
Erratic Flow/Pressure Reading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-18
4.7
Excessive System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-18
4.8
Peak “Ghosting” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-19
4.9
Nonreproducible Peak Height or Retention Time . . . . . . . . . . . . . . . .4-20
4.10
Abnormal Retention Time or Selectivity . . . . . . . . . . . . . . . . . . . . . .4-20
4.11
No Cell Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-20
4.12
High Cell Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-21
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ICS-2000 Ion Chromatography System
4.13
Baseline Noise or Drift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-22
4.14
Vacuum Degas Assembly Does Not Run . . . . . . . . . . . . . . . . . . . . . . 4-23
5 • Service 5.1
iv
Diagnostic and Calibration Procedures . . . . . . . . . . . . . . . . . . . . . . . . 5-1 5.1.1
Chromeleon Wellness Panel Overview . . . . . . . . . . . . . . . . . . 5-2
5.1.2
Diagnostic and Calibration Touch Screen Overview . . . . . . . 5-4
5.1.3
Calibrating the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . 5-5
5.1.4
Calibrating the Flow Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
5.1.5
Calibrating the Vacuum Degas Assembly . . . . . . . . . . . . . . . . 5-9
5.2
Isolating a Restriction in the Liquid Lines . . . . . . . . . . . . . . . . . . . . . 5-10
5.3
Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-14
5.4
Rebuilding the Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
5.5
Cleaning and Replacing the Pump Check Valves . . . . . . . . . . . . . . . 5-16
5.6
Replacing a Pump Piston Seal and Piston Rinse Seal . . . . . . . . . . . . 5-18
5.7
Replacing a Pump Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22
5.8
Replacing the Waste Valve or Priming Valve O-Ring . . . . . . . . . . . . 5-23
5.9
Replacing the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
5.10
Replacing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-28
5.11
Replacing the Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-29
5.12
Replacing the Column Heater Heat Exchanger . . . . . . . . . . . . . . . . . 5-32
5.13
Replacing the Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-33
5.14
Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-35
5.15
Priming the Pump with Isopropyl Alcohol . . . . . . . . . . . . . . . . . . . . . 5-36
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Contents
5.16
Changing Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-37
5.17
Replacing an EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-38 5.17.1 Replacing a KOH, LiOH, MSA, or NaOH EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-39 5.17.2 Replacing a K2CO3 Cartridge . . . . . . . . . . . . . . . . . . . . . . . .5-48
5.18
Replacing the CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-60
5.19
Replacing the EPM Electrolytic pH Modifier . . . . . . . . . . . . . . . . . . .5-64 5.19.1 Recording the EPM Serial Number in Chromeleon . . . . . . . .5-65 5.19.2 Plumbing the EPM for Hydrating and Conditioning . . . . . . .5-66 5.19.3 Hydrating and Conditioning the EPM . . . . . . . . . . . . . . . . . .5-68
5.20
Replacing the EGC CO3 Mixer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-69 5.20.1 Installing the New EGC CO3 Mixer . . . . . . . . . . . . . . . . . . .5-69 5.20.2 Filling the EGC CO3 Mixer with Deionized Water . . . . . . . .5-70 5.20.3 Filling the EGC CO3 Mixer with Eluent . . . . . . . . . . . . . . . .5-73
5.21
Replacing the EGC Holder and Degas Assembly . . . . . . . . . . . . . . . .5-80 5.21.1 Disconnecting and Removing the EluGen Cartridge . . . . . . .5-80 5.21.2 Removing the CR-TC and Reinstalling it in the New EGC Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-83 5.21.3 Removing the EPM and Reinstalling it in the New EGC Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-85 5.21.4 Installing the New EGC Holder without a CR-TC or EPM . .5-87 5.21.5 Reinstalling the EluGen Cartridge . . . . . . . . . . . . . . . . . . . . .5-88
A • Specifications A.1
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Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
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ICS-2000 Ion Chromatography System
A.2
Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1
A.3
Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1
A.4
Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2
A.5
Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2
A.6
Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-3
A.7
Conductivity Cell with Heat Exchanger . . . . . . . . . . . . . . . . . . . . . . . .A-3
A.8
Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-3
A.9
Vacuum Degas Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-3
A.10
Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-4
A.11
Eluent Generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-4
B • Installation
vi
B.1
Facility Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1
B.2
Unpacking the ICS-2000 System . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-2 B.2.1
Unpacking the Computer (North America only) . . . . . . . . . . .B-4
B.2.2
Unpacking the Computer (outside North America) . . . . . . . . .B-4
B.3
Installing Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-5
B.4
Installing the Chromeleon Software License . . . . . . . . . . . . . . . . . . . .B-6
B.5
Connecting the ICS-2000 to the Chromeleon PC . . . . . . . . . . . . . . . .B-10 B.5.1
Connecting the ICS-2000 to the PC . . . . . . . . . . . . . . . . . . . .B-10
B.5.2
Connecting Additional USB Devices. . . . . . . . . . . . . . . . . . .B-11
B.6
Connecting the Power Cord . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-12
B.7
Turning On the ICS-2000 Power . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-13
B.8
Setting Up Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-15
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B.9
B.10
B.8.1
Assigning the ICS-2000 to a Timebase. . . . . . . . . . . . . . . . . B-15
B.8.2
Assigning DX-LAN Devices to the Timebase (Optional) . . B-20
Installing and Plumbing the Columns and Suppressor . . . . . . . . . . . B-23 B.9.1
Setting Up the Column Heater . . . . . . . . . . . . . . . . . . . . . . . B-23
B.9.2
Installing the Columns. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-24
B.9.3
Installing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-25
Connecting the Waste Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-27 B.10.1 Installing the Gas Separator Waste Tube . . . . . . . . . . . . . . . B-27
B.11
Setting Up the Eluent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-29
B.12
Setting the Eluent Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-30
B.13
Priming the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-31 B.13.1 Priming the Eluent Lines with a Syringe . . . . . . . . . . . . . . . B-32 B.13.2 Priming the Pump Heads with the Prime Button . . . . . . . . . B-34
B.14
Setting Up the Eluent Generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-35 B.14.1 Eluent Generator Setup for KOH, LiOH, MSA, and NaOH Eluents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-36 B.14.2 Eluent Generator Setup for Carbonate/Bicarbonate Eluent . B-52 B.14.3 Eluent Generator Setup for Carbonate Eluent. . . . . . . . . . . . B-78
B.15
Setting Up a Chromeleon Application . . . . . . . . . . . . . . . . . . . . . . . B-95 B.15.1 Verifying Chromeleon Communication . . . . . . . . . . . . . . . B-104
B.16
Equilibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-105 B.16.1 EluGen Cartridge Backpressure Requirements. . . . . . . . . . B-106
B.17
Verifying Operational Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-106
B.18
Connecting an AS or AS50 (USB) Autosampler (Optional) . . . . . . B-107 B.18.1 AS or AS50 (USB) Connections . . . . . . . . . . . . . . . . . . . . . B-108
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ICS-2000 Ion Chromatography System
B.18.2 AS or AS50 (USB) Chromeleon Setup . . . . . . . . . . . . . . . .B-110 B.19
Connecting an AS40 Automated Sampler (Optional) . . . . . . . . . . .B-111
B.20
Connecting the Analog Output (Optional) . . . . . . . . . . . . . . . . . . . .B-113
B.21
Pressurizing the Eluent Reservoir (Optional) . . . . . . . . . . . . . . . . . .B-113 B.21.1 Connect the Gas Source . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-114 B.21.2 Pressurize the Eluent Reservoir . . . . . . . . . . . . . . . . . . . . . .B-115
B.22
Pump Continuous Seal Wash Connections (Optional) . . . . . . . . . . .B-116
B.23
Manually Connecting to a Control Panel . . . . . . . . . . . . . . . . . . . . .B-118
B.24
Installation Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-120
C • Touch Screen Operation C.1
Using the Touch Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-1
C.2
Using the Touch Screen with Chromeleon . . . . . . . . . . . . . . . . . . . . . .C-4
C.3
Overview of ICS-2000 Touch Screen Pages . . . . . . . . . . . . . . . . . . . .C-5
C.4
Home Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-6 C.4.1
Home Page Pump Controls . . . . . . . . . . . . . . . . . . . . . . . . . . .C-6
C.4.2
Home Page EGC Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-8
C.4.3
Home Page Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . .C-8
C.4.4
Home Page Injection Valve Controls . . . . . . . . . . . . . . . . . . . .C-9
C.4.5
Home Page Detector Controls . . . . . . . . . . . . . . . . . . . . . . . . .C-9
C.4.6
Other Home Page Controls. . . . . . . . . . . . . . . . . . . . . . . . . . .C-10
C.5
Plot Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-11
C.6
Status Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .C-12 C.6.1
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Viewing Other Status Parameters. . . . . . . . . . . . . . . . . . . . . .C-14
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C.6.2 C.7
C.8
Status Parameter Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-15
Pump Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-16 C.7.1
Setting Pump Pressure Limits and Selecting the Pressure Unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-16
C.7.2
Setting Degas Operating Parameters. . . . . . . . . . . . . . . . . . . C-17
C.7.3
Controlling the Eluent Valve. . . . . . . . . . . . . . . . . . . . . . . . . C-18
Eluent Generator Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-19 C.8.1
EGC Serial Number. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-19
C.8.2
Setting the Eluent Concentration. . . . . . . . . . . . . . . . . . . . . . C-20
C.8.3
Controlling the Eluent Generator Power . . . . . . . . . . . . . . . . C-21
C.8.4
Monitoring the EluGen Cartridge Life . . . . . . . . . . . . . . . . . C-21
C.8.5
Controlling the CR-TC Power. . . . . . . . . . . . . . . . . . . . . . . . C-22
C.9
Suppressor Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-23
C.10
Detector Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-24 C.10.1 Setting the Data Rise Time . . . . . . . . . . . . . . . . . . . . . . . . . . C-25 C.10.2 Selecting the Conductivity Polarity. . . . . . . . . . . . . . . . . . . . C-25 C.10.3 Setting Analog Out Options . . . . . . . . . . . . . . . . . . . . . . . . . C-26
C.11
Information Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-27
C.12
Module Setup Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-28
C.13
Input/Output Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-29
C.14
Diagnostic and Calibration Pages . . . . . . . . . . . . . . . . . . . . . . . . . . . C-30
D • TTL and Relay Control D.1
TTL and Relay Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-1 D.1.1
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ICS-2000 Ion Chromatography System
D.2
Controlling TTL and Relay Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . .D-5
D.3
Example Setup for Stand-Alone Operation . . . . . . . . . . . . . . . . . . . . .D-7
E • Reordering Information F • FAQ F.1
How do I hook up an autosampler? . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
F.2
How do I print? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
F.3
Why are the retention times moving? . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
F.4
How do I adjust retention times? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
F.5
When should I remake standards? . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
F.6
When should I replace the eluent generator cartridge? . . . . . . . . . . . . F-2
F.7
How do I start Chromeleon? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
F.8
How do I delete data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
F.9
How do I back up data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
F.10
How do I shut off the system? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
F.11
How do I store columns? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
F.12
How do I know when a column is dirty? . . . . . . . . . . . . . . . . . . . . . . . F-3
F.13
How do I clean a column? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-3
F.14
Why is the conductivity high? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-3
G • Glossary
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1.1
Introduction to Ion Chromatography (IC) The Dionex ICS-2000 Ion Chromatography System (ICS-2000) performs ion analyses using suppressed or non-suppressed conductivity detection. An ion chromatography system typically consists of a liquid eluent, a high-pressure pump, a sample injector, a guard and separator column, a chemical suppressor, a conductivity cell, and a data collection system. Before running a sample, the ion chromatography system is calibrated using a standard solution. By comparing the data obtained from a sample to that obtained from the known standard, sample ions can be identified and quantitated. The data collection system, typically a computer running chromatography software, produces a chromatogram (a plot of the detector output vs. time). The chromatography software converts each peak in the chromatogram to a sample concentration and produces a printout of the results.
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ICS-2000 Ion Chromatography System
A typical IC analysis consists of six stages (see Figure 1-1). 6. Data Analysis Conductivity Cell
5. Detection
Suppressor
1. Eluent Delivery
4. Suppression
Eluent Separator Column
3. Separation Pump
Guard Column
Injection Valve Sample
2. Sample Injection Sample Loop
Figure 1-1. Ion Analysis Process
1. Eluent Delivery
•
•
Eluent, a liquid that helps to separate the sample ions, carries the sample through the ion chromatography system. The ICS-2000 includes an eluent generator, which generates eluent online from deionized water. When the ICS-2000 is controlled from the front panel, only isocratic eluent delivery is possible. This means that the eluent composition and concentration remain constant throughout the run. Gradient delivery (a change in concentration over time) is possible when the ICS-2000 is controlled by Chromeleon® Chromatography Management System (the data collection system for the ICS-2000).
2. Sample Injection
•
1-2
The liquid sample is loaded into a sample loop either manually or automatically (if an automated sampler is installed). When triggered, the ICS-2000 injects the sample into the eluent stream.
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The pump pushes the eluent and sample through the guard and separator columns (chemically-inert tubes packed with a polymeric resin). The guard column removes contaminants that might poison the separator column.
3. Separation
•
As the eluent and sample are pumped through the separator column, the sample ions are separated. In the ICS-2000, the mode of separation is called ion exchange. This is based on the premise that different sample ions migrate through the IC column at different rates, depending upon their interactions with the ion exchange sites.
4. Suppression
•
After the eluent and sample ions leave the column, they flow through a suppressor that selectively enhances detection of the sample ions while suppressing the conductivity of the eluent.
5. Detection
•
A conductivity cell measures the electrical conductance of the sample ions as they emerge from the suppressor and produces a signal based on a chemical or physical property of the analyte.
6. Data Analysis
• •
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The conductivity cell transmits the signal to a data collection system. The data collection system (for the ICS-2000, this is Chromeleon) identifies the ions based on retention time, and quantifies each analyte by integrating the peak area or peak height. The data is quantitated by comparing the sample peaks in a chromatogram to those produced from a standard solution. The results are displayed as a chromatogram and the concentrations of ionic analytes can be automatically determined and tabulated.
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ICS-2000 Ion Chromatography System
1.2
Overview of the ICS-2000 The ICS-2000 is an integrated ion chromatography system containing an eluent generator, pump, injection valve, column heater, and conductivity detector. Other system components, including a guard column, separator column, and suppressor vary, depending on the analyses to be performed. The ICS-2000 is also configured with a vacuum degas assembly, for online eluent degassing. ICS-2000 operation can be controlled in one of two ways:
• •
Remotely, with a personal computer running Microsoft® Windows® XP or Windows 2000 and Chromeleon software (version 6.5 SP2 or later). Chromeleon also provides data acquisition and data processing functions. Locally, with the front panel LCD touch screen. The touch screen is used for instrument control only. It does not provide data acquisition or data processing functions. An analog output on the rear panel can be connected to a separate data acquisition device.
For communication between the ICS-2000 and Chromeleon, the ICS-2000 is connected to a USB (Universal Serial Bus) port on the computer or a USB hub. For installation instructions, see Section B.5 and also refer to Installing the Chromeleon Chromatography Management System with a Dionex Ion Chromatograph (IC) (Document No. 031883).
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1.3
About This Manual The electronic version (i.e., PDF file) of the ICS-2000 operator’s manual contains numerous hypertext links that can take you to other locations within the file. These links include:
•
Table of contents entries
•
Index entries
•
Cross-references (underlined in blue) to sections, figures, tables, etc.
If you are not familiar with how to navigate PDF files, refer to the Help system for Adobe® Acrobat® or Adobe Reader® for assistance Chapter 1 Introduction
Introduces ion analysis and the ICS-2000; explains the conventions used in this manual, including safety-related information.
Chapter 2 Features Overview
Provides an overview of ICS-2000 operating features and system components; introduces the Chromeleon user interface.
Chapter 3 Operation and Maintenance
Provides operating instructions and describes routine preventive maintenance procedures.
Chapter 4 Troubleshooting
Lists problems and presents step-by-step procedures for how to isolate and eliminate the cause of each problem.
Chapter 5 Service
Provides step-by-step instructions for routine service and parts replacement procedures that the user can perform.
Appendix A Specifications
Lists the ICS-2000 specifications and installation site requirements.
Appendix B Installation
Describes how to install the ICS-2000.
Chapter C Touch Screen Operation
Describes the operating features available from the front panel touch screen.
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ICS-2000 Ion Chromatography System
Appendix D TTL and Relay Control
Describes the ICS-2000 TTL and relay control features.
Appendix E Reordering Information
Lists spare parts for the ICS-2000.
Appendix F FAQ
Provides answers to frequently asked questions about ICS2000 operation.
Appendix G Glossary
Defines terms commonly used in ion analysis.
1.3.1
Safety Messages and Notes The ICS-2000 is designed for IC (ion chromatography) applications and should not be used for any other purpose. If there is a question regarding appropriate usage, contact Dionex at 1-800-346-6390 before proceeding. Outside the United States, call the nearest Dionex office. This manual contains warnings and precautionary statements that, when properly followed, can prevent personal injury and/or damage to the instrument. Safety messages appear in bold type and are accompanied by icons, as shown below. Indicates an imminently hazardous situation which, if not avoided, will result in death or serious injury.
Indicates a potentially hazardous situation which, if not avoided, could result in death or serious injury. Indicates a potentially hazardous situation which, if not avoided, may result in minor or moderate injury. Also used to identify a situation or practice that may seriously damage the instrument, but will not cause injury. Indicates that the function or process of the instrument may be impaired. Operation does not constitute a hazard.
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Messages d'avertissement en français Signale une situation de danger immédiat qui, si elle n'est pas évitée, entraînera des blessures graves à mortelles.
Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures graves à mortelles. Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures mineures à modérées. Également utilisé pour signaler une situation ou une pratique qui pourrait gravement endommager l'instrument mais qui n'entraînera pas de blessures.
Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen.
Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen. Bedeutet eine mögliche Gefährdung. Mißachtung kann zu kleineren oder mittelschweren Verletzungen führen. Wird auch verwendet, wenn eine Situation zu schweren Schäden am Gerät führen kann, jedoch keine Verletzungsgefahr besteht.
Notes
Informational messages also appear throughout this manual. These are labeled NOTE and are in bold type: NOTE NOTES call attention to certain information. They alert you to an unexpected result of an action, suggest how to optimize instrument performance, etc.
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ICS-2000 Ion Chromatography System
1.3.2
Safety Labels The TUV GS and c TUVus Mark safety labels and the CE Mark label on the ICS-2000 indicate that the ICS-2000 is in compliance with the following standards: EN 61010-1:2001 (safety), CAN/CSA-C22.2 No. 1010.1-92 +A2:97 (safety), UL 3101-1/10.93 (safety), and EN 61326:1997, including A1:1998 and A2:2001 (EMC susceptibility and immunity). The symbols below appear on the ICS-2000 or on labels affixed to the ICS-2000. Alternating current Protective conductor terminal (earth ground) Power supply is on Power supply is off
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2 • Features This chapter describes key ICS-2000 features and introduces the Chromeleon user interface.
2.1
Operating Features 2.1.1
Front Panel Figure 2-1 illustrates the front panel of the ICS-2000. Injection Port
Touch Screen Power LED
The sample to be analyzed can be injected manually into the injection port, using a syringe. For automated sample injection, the ICS-2000 must be connected to an autosampler. For more information about sample injection, see Section 3.10. Touch Screen
Injection Port
The LCD touch screen provides local control of most ICS-2000 functions. You can control many of these functions directly on the touch screen’s HOME page (see Figure 2-2). From the HOME page you can also go to a series of pages that provide access to all other locally controlled ICS-2000 operating functions.
Figure 2-1. ICS-2000 Front Panel
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ICS-2000 Ion Chromatography System
Summary of Touch Screen Operation
Status Field Edit Field
Command Button (selected) Command Button (unselected)
Figure 2-2. ICS-2000 Touch Screen Home
Page
NOTE To adjust the screen contrast, open the front door and adjust the knurled knob under the screen (see Figure 2-8).
• • •
Edit fields and command buttons have blue text on a shaded background. Fields that display status information are not shaded. Edit fields have square corners, while command buttons are rounded. To select a command button or edit a field, touch and release the command button or edit field with your fingertip.
NOTE When you touch a button or edit field, the action is taken when you lift your finger. If you unintentionally touch a button or field, you can cancel the action by sliding your finger away from the button or field before lifting.
•
2-2
Touching a command button (for example, command immediately.
) executes the
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2 • Features •
•
Selecting a command button changes the button’s appearance to white text on a dark backgound (for example, ). Touching an edit field (for example, ) opens a page with a number keypad (see Figure 2-3). Use the keypad to enter the desired numerical value for the field and then touch the ENTER button.
Touch CANCEL to cancel the entry and return to the previous page.
Touch a number to enter the value.
Touch ENTER to confirm the entry and return to the previous page.
Figure 2-3. Number Keypad
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ICS-2000 Ion Chromatography System •
Touching the page name (for example, ) in the bottom right corner opens a menu of pages (see Figure 2-4).
Touch a page name to display the page.
Figure 2-4. ICS-2000 Touch Screen Menu of Pages
•
2-4
Touching a page name on the menu of pages displays the selected page. For example, touching SUPPRESSOR displays the
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2 • Features
page (see Figure 2-5). See Appendix C for details about each touch screen page.
SUPPRESSOR
Touch to select a different option.
Touch to return to the Home page.
Figure 2-5. Suppressor Page
•
Touching
returns you to the HOME page.
•
Touching
opens a list of options (see Figure 2-6).
Touch an option to select it.
Figure 2-6. Suppressor Page: Selecting an Option
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ICS-2000 Ion Chromatography System
2.1.2
Top Cover Figure 2-7 illustrates the top cover of the ICS-2000. EluGen Cartridge and Holder
EluGen Cartridge and Reservoir Storage
The ICS-2000 top cover holds one or two EluGen® cartridges (see below) and up to two 2-L plastic reservoirs (P/N 044129).
Second EluGen Cartridge or Reservoir Area EluGen Cartridges EGC, EPM, and CR-TC Connectors Tubing Chase (under connectors)
EGC Service Area
Deionized Water
The EluGen cartridges are installed in holders that fit into the two back reservoir areas. See Section 2.4.4 for details about the eluent generator. Tubing Chase
4L Reservoir Area
The tubing chase under the EGC and CR-TC connectors routes tubing from the eluent reservoir and EGC holder to the front of the ICS-2000.
Figure 2-7. ICS-2000 (Top View) EGC, EPM, and CR-TC Connectors
The cable from the EluGen cartridge (EGC) connects to the EGC-1 connector. The cable from the Continuously Regenerated Trap Column (CR-TC) connects to the CR-TC connector. See Section B.14 for installation instructions. If a second EluGen cartridge is installed, it connects to the EGC-2 connector. When operating with an EGC II K2CO3 EluGen Cartridge and the EPM Electrolytic pH Modifier, the EluGen cartridge is typically connected to the EGC-1 connector. The pH modifier, which mounts on the side of the EluGen cartridge holder, is connected to the EGC-2 connector. However, the connections can be reversed, if desired.
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EGC Service Area
The EGC service area holds the cartridge during installation and replacement. See Section B.14 for instructions.
2.1.3
Component Panel Figure 2-8 shows the user-accessible components installed on the component panel behind the ICS-2000 front door.
11
10 9
6
1
Eluent Valve
2
Leak Sensor
3
Pump Heads
4
Pressure Transducer
5
Injection Valve
6
Column Heater and Columns
7
Suppressor
8
DS6 Cell
9
Mounting Brackets for a Second Suppressor
7 8
5
4
10 Screen Adjustment
3
Knob (under display)
11
1
2
11 Tubing Chase (2)
Figure 2-8. ICS-2000 Component Panel
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ICS-2000 Ion Chromatography System
Eluent Valve
The eluent valve controls the flow from the eluent reservoir. The eluent valve opens automatically when the pump is started and closes when the pump is turned off. Leak Sensor
The leak sensor is installed in the drip tray at the bottom of the component panel. If liquid accumulates in the tray, an error message is logged in the Chromeleon Audit Trail and displayed on the LCD touch screen. Pump Heads
The ICS-2000 includes a dual-piston serial pump. The flow rate can be set to 0.00 mL/min or to between 0.05 and 5.00 mL/min. However, for optimum performance, set the flow rate to between 0.40 and 2.00 mL/min. Setting the flow rate to 0.00 mL/min turns off the pump. See Section 2.4.3 for details about the pump. Pressure Transducer
The pressure transducer measures the system backpressure. Injection Valve
The injection valve is a six-port, electrically-activated valve. A 25-µL sample loop (P/N 042857) is installed on the valve at the factory. See Section 2.4.5 for details about valve operation. Separator and Guard Columns
Both the separator and guard columns are packed with resin and perform the separation of the sample ions. The main function of the guard column is to trap contaminants and remove particulates that might damage the separator column. Column Heater
The column heater controls the temperature of the separator and guard columns. The temperature can be set to between 30 and 60 °C, however it must be set at least 5 °C above the ambient temperature. See Section 2.4.6 for details about the column heater.
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Suppressor
The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an AES® Atlas Electrolytic Suppressor, SRS® Self-Regenerating Suppressor, or MMS™ MicroMembrane™ Suppressor can be used with the ICS-2000. See Section 2.4.7 for details about the suppressor. DS6 Heated Conductivity Cell
The flow-through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. A heat exchanger inside the cell regulates the temperature, which can be set to between 30 and 55 °C. For optimum performance, set the temperature to at least 7 °C above the ambient temperature. See Section 2.4.8 for details about the cell. Screen Adjustment Knob
Use this knob to change the LCD touch screen contrast. Tubing Chases
The upper tubing chase routes tubing from the top cover to the component panel. The lower tubing chase routes tubing from the component panel, through the ICS-2000 interior, to the rear panel.
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ICS-2000 Ion Chromatography System
2.1.4
Rear Panel Figure 2-9 illustrates the ICS-2000 rear panel.
Tubing Clips
Analog Output Connector Power Switch
USB Connectors
TTL and Relay Connector Strip
Main Power Receptacle
Waste Lines
Figure 2-9. ICS-2000 Rear Panel Analog Output Connector
The analog output connector outputs conductivity data (scaled to 1 volt) to an integrator or recording device. See Section B.20 for connection and setup information. USB Connectors
A USB receptacle is provided to allow connection to the Chromeleon computer. Two USB ports are provided for connecting to other USB devices. See Section B.5 for connection instructions.
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TTL and Relay Connector
The TTL and Relay connector strip provides two TTL outputs, two relay outputs, and four TTL inputs. The outputs can be used to control functions in other TTL- or relay-controllable devices. The inputs can be used to switch the injection valve position, turn on the pump, perform an autozero command, and send an event mark to the analog output. See Section D.1 for connection instructions. Tubing Clips
The tubing clips hold tubing routed from the top cover in place. Power Switch
The power switch provides on/off control of power to the ICS-2000. Main Power Receptacle
The power supply cord plugs into the AC power receptacle. The power supply cord is used as the main disconnect device. Make sure the socket-outlet is located near the ICS-2000 and is easily accessible. Le cordon d'alimentation principal est utilisé comme dispositif principal de débranchement. Veillez à ce que la prise de base soit située/installée près du module et facilement accessible. Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht zugänglich ist.
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ICS-2000 Ion Chromatography System
2.2
The Chromeleon Interface NOTE This section provides a brief overview of the Chromeleon interface. For details, refer to the Chromeleon Help or user’s manual.
Chromeleon software is used for remote control of ICS-2000 operation. Two modes of software control are available: direct control and automated control.
•
•
With direct control, you select operating parameters and commands from the Chromeleon menu bar, toolbars, and Control panels. Direct control commands are executed as soon as they are entered. Section 2.2.2 describes the commands available from the ICS-2000 Control panels. With automated control, you create a list of samples (a sequence) to be processed automatically. The sequence includes programs with commands and parameters for controlling the ICS-2000, acquiring sample data, and producing reports. Section 3.11.2 describes automatic sample processing.
2.2.1
The Chromeleon Main Window and Browser When you start Chromeleon, the main window and the Chromeleon Browser appear (see Figure 2-10).
Figure 2-10. Chromeleon Main Window and Browser
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NOTE The Chromeleon Browser looks and functions like Windows Explorer, but do not confuse the two. If you copy files from the Chromeleon Browser into Explorer, the files will be corrupted.
The Browser displays the directories in which chromatographic data is located, and allows you to open, move, and delete data.
•
•
2.2.2
The left pane of the Browser shows the directory tree structure. By clicking the ‘+’ signs next to the folders and expanding the directory tree, you can access sequences, System Control panels, Wellness Panels, and reports. The right pane displays information about the item selected in the left pane.
The ICS-2000 Control Panels Chromeleon provides two types of Control panels for the ICS-2000.
• •
System Control panels are used for controlling and monitoring ICS2000 operation. System Control panels are described below. The Wellness Panel is used for performing calibration and diagnostic functions. The Wellness Panel is described in Section 5.1.
System Control Panels
System Control panels for the ICS-2000 are located in the Dionex Templates/Panels/Dionex_IC\ICS-2000 folder. Chromeleon provides panels for each ICS-2000 system configuration. There are two styles of panels:
• •
Traditional system panels (see Figure 2-11) provide controls on a single window with minimal graphics. System panels (see Figure 2-12) provide a more graphical interface than the traditional style. On these panels, clicking a control often brings up another window in which you enter a value.
When you open a System Control panel, select a panel that matches your system configuration and choose the style that you prefer.
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ICS-2000 Ion Chromatography System
Figure 2-11. ICS-2000 System Control Panel (Traditional)
Figure 2-12. ICS-2000 System Control Panel (Graphical)
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System Controls Overview
This section provides brief descriptions of the various controls available on the ICS-2000 System Control panels. Sample Controls
Datasource
Displays the database in which the chromatographic data for the sample is saved. Sequence
Displays the sequence in which this sample is included. Sample
Displays the name of the sample that is running. Program
Displays the name of the program that is running. Elapsed Program Time
Displays the time that has elapsed since the sample analysis began. Total Program Time
Displays the total run time specified in the program.
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ICS-2000 Ion Chromatography System
Audit Trail
The Audit Trail displays an account of every event that occurs during ICS-2000 operation. This includes errors, status messages, operational events, etc. System Controls
Connected
Connects the ICS-2000 to the Chromeleon Control panel, enabling communication between the PC and the module. Clearing the check box disconnects the ICS-2000 from the PC. Startup
Starts the pump, suppressor, and eluent generator. The flow rate, suppressor current, and eluent concentration settings that were in effect at system shutdown (see below) are restored. Shutdown
Stops the pump, suppressor, and eluent generator. The flow rate, suppressor current, and eluent concentration settings currently in effect are remembered and will be restored at system startup (see above). Show Plot…
Displays the ICS-2000 detector signal plot in a separate window.
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Pump Controls
Flow Rate
Sets the pump flow rate in mL/min. Eluent Bottle
The entry field and gauge indicate the level of liquid (in liters) in the eluent bottle. This is a user-controlled feature. The level must be entered by the user when the reservoir is filled. See Section 3.4.2 for details. Off, On, Prime
Turn the pump on and off, or start the pump priming function. Eluent Flow Valve
Select the eluent flow valve position (Closed or Open). Max. Pressure
Displays the upper pressure limit. If this limit is exceeded, Chromeleon stops the flow, displays an error message, and stops the sample batch, as necessary. Curr. Pressure
Displays the current pressure. Min. Pressure
Displays the lower pressure limit. If this limit is exceeded, Chromeleon stops the flow, displays an error message, and stops the sample batch, as necessary.
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ICS-2000 Ion Chromatography System
Injection Valve Controls
LoadPosition InjectPosition
Displays the current position of the injection valve. Load
Switches the valve to the load position. Inject
Switches the valve to the inject position. Injection Valve Switch
Switches the valve from the current position to the other position. Column Heater Controls
Temperature
Displays the current heater temperature and lets you set a new temperature. Set Temp
Displays the current set temperature. Off
Turns the column heater off.
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Detector Controls
Autozero
Sets the conductivity to zero. Acq. Ready
Indicates whether the detector is ready to begin data acquisition. Total Cond
Displays the total conductivity (the conductivity including the offset conductivity). To determine the offset, allow the system to equilibrate after startup. At equilibration, the total conductivity is the background conductivity (the eluent conductivity before sample injection). Touch Autozero to zero the conductivity and offset this background reading from the total reading. Signal
Displays the offset conductivity (the total conductivity with the background conductivity subtracted). Data Rate
Sets the rate at which data points are recorded. Cell Temp
Sets the temperature of the cell. Supp. Type
Selects the type of suppressor installed. Supp. Current
Sets the current supplied to the suppressor. Supp. Mode
Turns the suppressor on or off.
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ICS-2000 Ion Chromatography System
Signal Plot
Displays a plot of the detector signal. Right-click to select plot options from a context menu. You can select autoscale commands, change the plot appearance, or select other signals to be displayed (for example, total conductivity or pump pressure). Eluent Generator Controls (Single Cartridge)
Concentration
Sets the concentration of eluent generated. On/Off
Turns the eluent generator on or off. Cartridge No.
Displays the serial number of the installed cartridge.
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Exp. Date
Displays the expiration date of the installed cartridge. Although you can continue operation with the cartridge after the expiration date, performance may be impaired until a new cartridge is installed. Cartridge Type
Displays the type of cartridge installed. Remaining Life
Displays the percentage of ions remaining in the cartridge. The ion percentage is counted down in 1% increments. Warning messages are displayed in the Chromeleon Audit Trail when the percentage falls below 30%. At 0%, an error message informs you that the ion count is depleted and the cartridge must be replaced before continuing operation. Normalized Life (displayed when an EPM is installed) Indicates how much the EPM has been used. The value starts at 0 and counts up with use. A count of 1 means the EPM usage is approximately equal to the lifetime of one K2CO3 cartridge. CR-TC
Turns the CR-TC on or off. Eluent Generator Controls (Dual Cartridge)
Dual panels provide controls for either two EluGen cartridges or for one EluGen cartridge and one EPM. For carbonate/bicarbonate eluent generation, the K2CO3 cartridge is typically connected to EGC-1 and the EPM is connected to EGC-2. Except for the following two controls, the
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ICS-2000 Ion Chromatography System
controls for each cartridge in the dual panel are the same as described for the single cartridge panel controls (see page 20). Target Concentration
Sets the concentration of eluent generated. If a K2CO3 EluGen cartridge and an EPM Electrolytic pH Modifier are installed (connected to EGC-1 and EGC-2, respectively), set the EGC-1 Target Concentration to the concentration of K2CO3 required for your application and set the EGC2 Target Concentration to the concentration of KHCO3 required. Applied Concentration
Displays the concentration of eluent currently being generated. For carbonate/bicarbonate eluent, the Applied Concentration for the K2CO3 cartridge is equal to the total of the target concentrations from both cartridges. This is the actual concentration of K2CO3 that the cartridge must generate in order to achieve the desired K2CO3/KHCO3 eluent mixture: Applied Concentration K2CO3 = Target Concentration K2CO3 + Target Concentration EPM
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2.3
Flow Schematics The following figures illustrate the liquid flow path through an ICS-2000 when using suppression in autorecycle mode. Three configurations are shown:
•
•
•
Figure 2-13 illustrates the liquid flow path when the components required for producing KOH, LiOH, MSA, or NaOH eluent are installed. The required components include the corresponding type of EluGen cartridge and a CRTC. Figure 2-14 illustrates the liquid flow path when the components required for producing carbonate/bicarbonate eluent are installed. The required components include an EGC II K2CO3 EluGen Cartridge, an EPM Electrolytic pH Modifier, and an EGC CO3 Mixer. Figure 2-15 illustrates the liquid flow path when the components required for producing carbonate eluent are installed. The required components include an EGC II K2CO3 EluGen Cartridge and an EGC CO3 Mixer.
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ICS-2000 Ion Chromatography System
To the pump Degas In EGC Vent
6
EGC II KOH, LiOH, MSA, or NaOH
1
Deionized Water
Inlet
Outlet
Regen In
8
Regen Out
Eluent
7
EGC Degas
Eluent Out
16 CR-TC
17
From the pulse damper
Degas In
To the inject valve port P(2)
Column Heater Degas Out
13
Suppressor
Cell Out
15
Eluent Out
Regen In
14
Heat Exchanger
Conductivity Cell Cell In
5
Pulse Damper Valve 10
W
Press. 4 Xducer. C
P
L
9
3 12
To waste
Eluent Valve
Pump Head
Guard
Pump Head
2
Sample in
Separator
Backpressure Coil
11
L
S
To waste
18
To Gas Separator Assembly
Figure 2-13. ICS-2000 Flow Schematic: KOH, LiOH, MSA, or NaOH Eluent Generation
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Flow Description for KOH, LiOH, MSA, or NaOH Eluent Generation
Refer to Figure 2-13 for the flow path number locations.
•
Deionized water from the reservoirn flows first through the pump degas assembly and then through the eluent valveo to the pumpp . The water is then pushed through the pressure transducerq, which measures the system pressure. From there, the water flows through a pulse damperr , which smooths minor pressure variations from the pump to minimize baseline noise.
•
Water then flows into the EluGen cartridge (EGC)s , which generates the programmed concentration of eluent. Eluent exits the cartridge and flows through the CR-TCt (which traps ionic contaminants), through the EGC degas tubing assemblyu, and on to the injection valvev.
•
After sample is loaded into the sample loopw and the injection valve is toggled to the Inject position, eluent passes through the sample loop.
• • • •
The eluent/sample mixture is pumped through the heat exchanger 11 , which heats the mixture to the column heater temperature. The mixture then goes to the guard and separator columns 12 and through the suppressor 13 . From the suppressor, the mixture flows through the cell 14 , where the analytes are detected. A digital signal is sent to Chromeleon software. Analog output can be collected simultaneously. The mixture flows out of the cell and is recycled back into the suppressor 15 , where it is the water source for the regenerant chamber. Regenerant waste from the suppressor is directed back to the CR-TC 16 , and then to the EGC degas tubing 17 , where any released hydrogen or oxygen gas is removed before it is sent to the gas separator assembly and then to waste 18 .
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ICS-2000 Ion Chromatography System
To the pump Degas In EGC Vent 6
EGC II K2CO3
1
Deionized Water
Inlet
Outlet Eluent Out
8
7
Regen Out
EGC Degas
Eluent In
18
EPM
Regen In
17
Degas In
14
Suppressor
Cell Out
16
Eluent Out
Regen In
15
Heat Exchanger
Regen Out
Eluent In
Degas Out Conductivity Cell Cell In
Column Heater
9
Pulse Damper Valve
L
Press. 4 Xducer.
C P
10
Separator
11
W
12
L
S
13
3
EGC CO3 Mixer
5
19
To waste Pump Head
Guard
Pump Head
To Gas Separator Assembly
2
Sample in
To waste
Eluent Valve
Backpressure Coil
Figure 2-14. ICS-2000 Flow Schematic: Carbonate/Bicarbonate Eluent Generation
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Flow Description for Carbonate/Bicarbonate Eluent Generation
Refer to Figure 2-14 for the flow path number locations.
•
Deionized water from the reservoirn flows first through the pump degas assembly and then through the eluent valveo to the pumpp . The water is then pushed through the pressure transducerq, which measures the system pressure. From there, the water flows through a pulse damperr , which smooths minor pressure variations from the pump to minimize baseline noise.
•
Water then flows into the EluGen cartridge (EGC)s , which generates the programmed concentration of carbonate eluent. Eluent exits the cartridge and flows through the EPMt, which adjusts the eluent concentration to produce the carbonate/bicarbonate mixture. The mixture flows through the EGC degas tubing assemblyu to the EGC CO3 Mixerv (to ensure a homogenous carbonate/bicarbonate mixture), and then on to the injection valvew.
• • • • •
After sample is loaded into the sample loop 11 and the injection valve is toggled to the Inject position, eluent passes through the sample loop. The eluent/sample mixture is pumped through the heat exchanger 12 , which heats the mixture to the column heater temperature. The mixture then goes to the guard and separator columns 13 and through the suppressor 14 . From the suppressor, the mixture flows through the cell 15 , where the analytes are detected. A digital signal is sent to Chromeleon software. Analog output can be collected simultaneously. The mixture flows out of the cell and is recycled back into the suppressor 16 , where it is the water source for the regenerant chamber. Regenerant waste from the suppressor is directed back to the EPM 17 , and then to the EGC degas tubing 18 , where any released hydrogen or oxygen gas is removed before it is sent to the gas separator assembly and then to waste 19 .
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ICS-2000 Ion Chromatography System
To the pump Degas In EGC Vent 6
EGC II K2CO3
1
Deionized Water
Inlet
Outlet
7 EGC Degas 16
Degas In
13
Suppressor
Cell Out
15
Eluent Out
Regen In
14
Heat Exchanger
Conductivity Cell Cell In
Regen Out
Eluent In
Degas Out
Column Heater
8
11
L
10
W L
Separator
Pulse Damper Valve
S
Press. 4 Xducer.
C P
12
3
9 Pump Head
2
Sample in To waste
Eluent Valve
Backpressure Coil
To waste Guard
Pump Head
EGC CO3 Mixer
5
17
To Gas Separator Assembly
Figure 2-15. ICS-2000 Flow Schematic: Carbonate Eluent Generation
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Flow Description for Carbonate Eluent Generation
Refer to Figure 2-15 for the flow path number locations.
•
Deionized water from the reservoirn flows first through the pump degas assembly and then through the eluent valveo to the pumpp . The water is then pushed through the pressure transducerq, which measures the system pressure. From there, the water flows through a pulse damperr , which smooths minor pressure variations from the pump to minimize baseline noise.
•
Water then flows into the EluGen cartridge (EGC)s , which generates the programmed concentration of carbonate eluent. Eluent exits the cartridge and flows through the EGC degas tubing assemblyt. Eluent then goes to the EGC CO3 Mixeru (to ensure a homogenous eluent concentration), and then on to the injection valvev.
•
After sample is loaded into the sample loopw and the injection valve is toggled to the Inject position, eluent passes through the sample loop.
• • • •
The eluent/sample mixture is pumped through the heat exchanger 11 , which heats the mixture to the column heater temperature. The mixture then goes to the guard and separator columns 12 and through the suppressor 13 . From the suppressor, the mixture flows through the cell 14 , where the analytes are detected. A digital signal is sent to Chromeleon software. Analog output can be collected simultaneously. The mixture flows out of the cell and is recycled back into the suppressor 15 , where it is the water source for the regenerant chamber. Regenerant waste from the suppressor is directed back to the EGC degas tubing 16 , where any released hydrogen or oxygen gas is removed before it is sent to the gas separator assembly and then to waste 17 .
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ICS-2000 Ion Chromatography System
2.4
System Component Details This section provides details about ICS-2000 system components, including the vacuum degas assembly, pump, eluent generator, injection valve, column heater, suppressor, and conductivity cell.
2.4.1
Vacuum Degas Assembly The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user. The assembly, which must be installed in the ICS-2000 at the factory, consists of:
•
A single-channel degas chamber (with degas membranes) with internal capacity of 17 mL
•
A dual-stage diaphragm vacuum pump
•
A solenoid valve
•
An on-board vacuum sensor
•
The electronics required to operate the vacuum pump
•
Tubing, fittings, and other accessories
By default, the ICS-2000 monitors the degas pressure reading and turns the degas pump on and off as needed. A different degas operating mode can be selected from the touch screen PUMP page (see Section C.7) or from Chromeleon. To select degas operating options from Chromeleon, open the Server Configuration program, select the ICS-2000 device icon
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under the timebase, and select Edit>Properties. Select the Options tab (see Figure 2-16).
Figure 2-16. Server Configuration Properties: Degas Mode Options Degas Mode Options
•
Always Off: The degas pump is always off.
•
Always On: The degas pump is always on. This setting is for test
purposes by a Dionex Service Representative. Do not use this setting for routine operation.
•
Cycle: The degas pump cycles on and off according to the times specified in the Cycle On and Off fields. Cycle On specifies for how long the degas pump runs during a cycle. Cycle Off specifies the time
between cycles.
•
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Monitor: (default mode) The ICS-2000 monitors the degas pressure reading and turns the degas pump on and off as required.
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ICS-2000 Ion Chromatography System
2.4.2
Eluent Valve The eluent valve controls the flow from the eluent reservoir. The valve opens automatically when the pump is started and closes when the pump is turned off. The valve can also be opened and closed manually either from the Chromeleon Control panel (see Section 2.2.2), or the touch screen PUMP page (see Section C.7). This lets you perform service procedures on pump components without eluent leaks occurring. Figure 2-17. Eluent Valve
2.4.3
Pump The ICS-2000 pump is a microprocessor-based isocratic eluent delivery system. Its variable speed, dual-piston series design ensures pulse-free pumping for the most demanding applications. Primary Pump Head
The primary pump head pumps eluent into the secondary head (see Figure 2-18). The check valves, which prevent reverse flow through the pump, are located on the bottom (inlet) and top (outlet) of the primary pump head. The priming valve is on the front of the pump head.
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Outlet Check Valve
Pressure Transducer
Primary Pump Head Secondary Pump Head
Priming Valve Inlet Check Valve
Waste Valve
Figure 2-18. ICS-2000 Pump Components
To open the priming valve, turn the knob one-quarter to one-half turn counterclockwise. When the priming valve is open, liquid can flow into and out of the primary pump head via the port in the front of the valve. NOTE The priming valve must be open when the pump is being primed with a syringe or with isopropyl alcohol. For detailed priming instructions, see Section B.13. Secondary Pump Head
The secondary pump head delivers eluent to the remainder of the chromatography system (the injection valve, column, and detector). The waste valve is located on the front of the secondary pump head (see Figure 2-18). To open the waste valve, turn the knob one-quarter to one-half turn counterclockwise. When the waste valve is in the open position, all output is directed to waste. NOTE The waste valve must be open when the pump is being primed using the Prime button. For detailed priming instructions, see Section B.13.
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ICS-2000 Ion Chromatography System
Pressure Transducer
Flow exiting the secondary pump head is directed to the pressure transducer (see Figure 2-18), which measures the system pressure. Pressure readings indicate that the pumping system is delivering smooth, accurate flow. Pressure readings can be monitored from the Chromeleon Control panel or the touch screen HOME page. The system pressure should remain consistent (no more than a 3% difference from one pressure reading to the next). High and low pressure limits can be used to stop the pump flow if a limit is exceeded. The pressure limits can be set from Chromeleon (in the Server Configuration or in the control program) or from the touch screen PUMP page (see Section C.7). See Section 4.1 for troubleshooting information if a pressure limit is exceeded. Pulse Damper
Flow output from the pressure transducer continues to the pulse damper, which smooths minor pressure variations. From there, flow is directed to the injection valve and then to the remainder of the chromatography system. Piston Seal Wash
The pump includes a piston seal wash assembly that can be set up to continuously rinse the back of the piston seals to remove salt crystals and prolong the life of the seals. To use this feature, an external water source must be connected. See Section B.22 for connection instructions. For continued protection of the pump, replace the piston rinse seals (see Section 5.6) and O-rings in the seal wash assembly every 6 months, or whenever you replace the main piston seals for the ICS-2000 pump.
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2.4.4
Eluent Generator The eluent generator produces high-purity eluents online, using only deionized water as the carrier. The eluent generator consists of an eluent generator cartridge (EGC) that generates the eluent, and a high-pressure degas tubing assembly that removes electrolysis gases created during eluent generation. NOTE A gas separator waste tube (P/N 045460) should be connected to the system waste line during installation (see Section B.10.1).
Several types of EluGen cartridges are available for use with the ICS2000 (see Table 2-1). Each cartridge contains 900 mL of the appropriate electrolyte concentrate solution for eluent generation. EluGen Cartridge
Part Number
Function
EGC II K2CO3 EluGen Cartridge
058904
EGC II KOH EluGen Cartridge EGC II LiOH EluGen Cartridge
058900
EGC II MSA EluGen Cartridge
058902
EGC II NaOH EluGen Cartridge
058908
Generates carbonate eluent for anion exchange separations. Note: Produces a carbonate/bicarbonate mixture when installed with the EPM Electrolytic pH Modifier (P/N 063175) and EGC CO3 Mixer (P/N 061686). Generates hydroxide eluent for anion exchange separations. Generates lithium hydroxide eluent for anion exchange separations. Generates methanesulfonic acid eluent for cation exchange separations. Generates sodium hydroxide eluent for anion exchange separations.
058906
Table 2-1. EluGen Cartridge Types for the ICS-2000
For more information, refer to the EluGen cartridge manual. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).
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ICS-2000 Ion Chromatography System
You can select the concentration of eluent to be generated from either the Chromeleon Control panel or from the touch screen HOME page (see Section C.4). The allowable eluent concentration depends on several factors: the flow rate, suppressor type, EluGen cartridge type, and cartridge configuration. For details, refer to Table 2-1 and Table 2-2. Single-Cartridge Configuration
In the single-cartridge configuration, the ICS-2000 contains one EluGen cartridge. EluGen Cartridge
Eluent Concentration Range
K2CO3
0.1 to 15 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 2.0 mL/min flow where X = 15/flow in mL/min
KOH
0.1 to 100 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 100/flow in mL/min
LiOH
0.1 to 80 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 80/flow in mL/min
MSA
0.1 to 100 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 100/flow in mL/min
NaOH
0.1 to 100 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 100/flow mL/min
Table 2-1. Eluent Concentration Ranges for Single-Cartridge Configurations Linked Dual-Cartridge Configuration
In the linked dual-cartridge configuration, the ICS-2000 contains two EluGen cartridges (or one EluGen cartridge and an EPM) that perform as one cartridge. Note that the allowable eluent concentration for a linked cartridge is less than when the cartridge is defined as independent. For
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details, refer to the EluGen cartridge manual. Cartridge manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). EluGen Cartridges
Eluent Concentration Range
Comment
K2CO3/EPM Electrolytic pH Modifier
0.1 to 15 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 2.0 mL/min flow X = 15/flow
The total of the eluent concentrations from both the EluGen cartridge and the EPM must not exceed the specified range. The EPM concentration must not exceed 10 mM. See “Generating Carbonate/Bicarbonat e Eluent” on page 239 for details.
KOH/KOH KOH/MSA KOH/NaOH MSA/MSA MSA/NaOH NaOH/NaOH
0.1 to 50 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.0 mL/min flow X = 50/flow
The eluent concentration range for each cartridge is cut by 50%.
LiOH/LiOH
0.1 to 40 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.0 mL/min flow X = 40/flow
The eluent concentration range for each cartridge is cut by 50%.
Table 2-2. Eluent Concentration Ranges for Linked Dual-Cartridge Configurations EluGen Cartridge Holder
The EluGen cartridge is installed in a cartridge holder, which mounts on the ICS-2000 top cover (see Figure 2-7). The cartridge holder also houses the high-pressure degas tubing assembly. The ICS-2000 can control up to two EluGen cartridges. However, when operating with an EGC II K2CO3 EluGen Cartridge and the pH Modifier,
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ICS-2000 Ion Chromatography System
only one cartridge can be installed, because the pH Modifier must be connected to the other EGC power supply (EGC-1 or EGC-2). Tubing and fittings for plumbing the cartridge, degas assembly, CR-TC, and EPM are included with the holder. See Section B.14 for installation instructions. Backpressure Coil (Optional)
The EluGen cartridge requires at least 14 MPa (2000 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. A system backpressure of 16 MPa (2300 psi) is ideal. If necessary, increase the system backpressure by installing a backpressure coil between the injection valve and the EluGen cartridge OUTLET port. For details, refer to Section B.16.1. Continuously Regenerated Trap Column (CR-TC)
The CR-TC is a high pressure electrolytically-regenerated trap column. The CR-TC is designed to remove anionic or cationic contaminants in the eluent or deionized water and to reduce drift during gradient separations. Two versions of the CR-TC can be used with the ICS-2000:
• •
CR-ATC (Continuously Regenerated Anion Trap Column, P/N 060477) CR-CTC (Continuously Regenerated Cation Trap Column, P/N 060478)
For more information, refer to the CR-TC manual. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891). NOTE The IonPac® ATC-HC Trap Column (P/N 059604) or IonPac CTC-1 Trap Column (P/N 040192) can be used with the ICS-2000. However, both IonPac trap columns require off-line chemical regeneration. Contact Dionex for more information.
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EPM Electrolytic pH Modifier and EGC CO3 Mixer
The EGC II K2CO3 EluGen Cartridge can be used with an EPM Electrolytic pH Modifier (P/N 063175) (see Figure 2-19) and an EGC CO3 Mixer (P/N 061686) to produce a carbonate/ bicarbonate mixture. The carbonate/bicarbonate mixture is used with carbonatebased IonPac columns for anion exchange separations.
EluGen Cartridge EPM
Figure 2-19. ICS-2000 with an EluGen Cartridge and EPM Installed
After the cartridge generates carbonate eluent, the pH Modifier adjusts the eluent concentration to produce the carbonate/bicarbonate mixture. The EGC CO3 Mixer provides enough mixing to produce a homogenous solution of electrolytically-generated K2CO3 and KHCO3 eluent. For more information about these products, refer to the EluGen cartridge manual. Cartridge manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). Generating Carbonate/Bicarbonate Eluent
If a K2CO3 EluGen cartridge and an EPM Electrolytic pH Modifier are installed (connected to EGC-1 and EGC-2, respectively), set EGC-1 to the concentration of K2CO3 required for your application and set EGC-2 to the concentration of KHCO3 required. In order to achieve the desired K2CO3/KHCO3 eluent mixture, the K2CO3 cartridge must generate the total of the two setpoint concentrations. For example, for a 3.50 mM K2CO3/1.00 mM KHCO3 eluent, set EGC-1 to 3.50 mM and EGC-2 to 1.00 mM. When the eluent is generated, the K2CO3 cartridge generates 4.50 mM K2CO3, which is then modified by the EPM to achieve the desired 3.50 mM K2CO3/1.00 mM KHCO3 mixture.
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2.4.5
Injection Valve The injection valve (P/N 057968) is a six-port, electrically-activated valve. A 25-µL sample loop (P/N 042857) is installed on the valve at the factory. The valve has two operating positions: Load and Inject (see Figure 2-20). LOAD POSITION
Sample In
Sample In
INJECT POSITION
To Column
To Column Sample Loop
To Waste
Sample Loop
From Pump
To Waste
From Pump
Figure 2-20. Injection Valve Flow Schematics
Eluent flows through either the Load or Inject path, depending on the valve position.
•
•
In the Load position, sample is loaded into the sample loop, where it is held until injection. Eluent flows from the pump, through the valve, and to the column, bypassing the sample loop. Sample flows from the syringe or automated sampler line (if installed), through the valve, and into the sample loop. Excess sample flows out to waste. In the Inject position, sample is swept to the column for analysis. Eluent flows from the pump, through the sample loop, and on to the column, carrying the contents of the sample loop with it. Section 3.10 describes how to inject samples.
Figure 2-21 shows the injection valve connections. The injection valve is plumbed at the factory with all tubing and fittings for connection to the pump, injection port, column, and waste. A 25-µL PEEK sample loop (P/N 042857) is installed between ports L (1) and L (4). Dionex offers
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sample loops in various sizes. If necessary, the pre-installed 25-µL loop can be replaced with a loop that has a different sample injection volume.
Figure 2-21. Injection Valve Plumbing NOTE The EluGen cartridge requires at least 14 MPa (2000 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. A system backpressure of 16 MPa (2300 psi) is ideal. If the system backpressure is too low, install a backpressure coil. Connect one end of the backpressure coil to Port P (2) on the injection valve; connect the other end to the TO INJ VALVE IN - P line. See Section B.16.1 for details.
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ICS-2000 Ion Chromatography System
2.4.6
Column Heater The column heater provides temperature control for the separator and guard column. The heater temperature can be set to between 30 and 60 °C. However, the set temperature must be at least 5 °C above the ambient temperature. A thermistor mounted in the heater block monitors the temperature. Setting the temperature to 0 °C turns off the column heater. If the temperature exceeds 65 °C, the column heater is shut off and the error message “Column heater exceeds safe temperature.” is displayed on the touch screen and in the Chromeleon Audit Trail. See Section 4.1 for troubleshooting information.
Figure 2-22. Column Heater
2.4.7
Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an Atlas Electrolytic Suppressor, Self-Regenerating Suppressor, or MicroMembrane Suppressor can be used with the ICS-2000. For details about any of the suppressors or for information about selecting a suppressor for your application, refer to the suppressor manuals. The manuals are on the Dionex Reference Library CD-ROM (P/N 053891).
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2.4.8
DS6 Heated Conductivity Cell The ICS-2000 flow-through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. Two passivated 316 stainless steel electrodes are permanently sealed into the PEEK cell body. The cell design provides efficient sweep-out, low volume (1 µL), and low dispersion. Temperature control and compensation help ensure good peak reproducibility and baseline stability. Temperature Control
Temperature directly affects the conductivity of a solution. For example, laboratory heating and air conditioning systems can cause a regular slow cycling in the baseline. This, in turn, can affect the reproducibility of an analysis. The higher the conductivity, the more pronounced the effect. In ion analysis, the effect of temperature variation is minimized by suppressing eluent conductivity. To further reduce the effect of temperature variation, a heater inside the cell regulates the ttemperature. The cell heater can be set to between 30 °C and 55 °C. The set temperature must be at least 7 °C above the ambient temperature. Setting the cell temperature to 0 °C turns off the cell heater. Temperature Compensation
Built-in preset temperature compensation of 1.7% per °C helps minimize changes in the baseline or in peak heights when the operating temperature is different from the temperature at which the cell was calibrated. DS6 Heated Conductivity Cell Components
The cell front cover provides CELL IN and CELL OUT fittings for connecting the cell to the suppressor (see Figure 2-8). The remaining cell components are mounted behind the component panel. To replace, the cell remove the screws on the cell front cover and pull the entire cell assembly out through the component panel. See Section 5.9 for cell replacement instructions.
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3 • Operation and Maintenance This chapter describes routine operating and maintenance procedures for the ICS2000 Ion Chromatography System. The ICS-2000 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of the ICS-2000 in a manner not specified by Dionex may result in personal injury.
3.1
Operation Overview Figure 3-1 illustrates the basic steps for routine operation of the ICS-2000.
Power up the system Start Chromeleon
Set up the reservoir Check all connections Prime the pump Set operating conditions Equilibrate the system Prepare samples Verify operating status Process samples
Figure 3-1. ICS-2000 Operation Flow Chart
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ICS-2000 Ion Chromatography System
Sample Processing Overview
Samples can be run manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-2 shows the typical steps for manual and batch sample processing.
Manual Sample Processing Using the Front Panel
Manual Sample Processing Using Chromeleon
Batch Sample Processing Using Chromeleon
Load the sample
Load the sample
Create a sequence (Sequence Wizard)
Autozero
Start data acquisition
Inject the sample
Autozero
Add the sequence to the batch
Start the batch (Optional) Record data from the analog output*
*A third-party recording
Inject the sample
Stop data acquisition
device must be connected to the analog output.
(Optional) Save the manual sequence data
Figure 3-2. Sample Processing Overview
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3.2
Power Up the System Press the power switch on the ICS2000 rear panel (see Figure 3-3) to turn on the system power. Table 3-2 shows the ICS-2000 conditions at power up.
Power Switch
Also turn on the power to the computer and the autosampler (if used).
Figure 3-3. ICS-2000 Rear Panel Feature
Power-Up Condition
Pump
Off
Injection valve
Load position
Cell
Reading current value
Suppressor
Off*
Cell heater
Set to the last value used. The default when the ICS-2000 is turned on for the first time is 35 °C.
Column oven temperature
Set to the last value used. The default when the ICS-2000 is turned on for the first time is 30 °C.
Eluent generator
Off*
CR-TC
Off
EPM
Off* Table 3-2. ICS-2000 Power-Up Conditions
* When you start the suppressor, eluent generator, or EPM, the value used last is restored.
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3.3
Start Chromeleon NOTE If you are beginning operation of an ICS-2000 that has not been configured in a timebase, see Section B.8 for Chromeleon setup instructions.
1. If the Chromeleon Server is not running (the icon on the taskbar is crossed out in red
), start the Server by right-clicking the icon and selecting Start
Server. When the server starts, the icon changes to gray
.
2. Start Chromeleon by selecting Start>Programs>Chromeleon> Chromeleon. The Chromeleon main window and the Browser will open. Your screen display should resemble Figure 3-4. If the Browser does not open, select File>Browser to open it.
Figure 3-4. Chromeleon Main Window and Browser
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3. In the Browser, expand the Dionex Templates\Panels\Dionex_IC\ICS-2000 System Panels folder. Several ICS-2000 Control panels (.PAN files), corresponding to various system configurations, are provided. Two styles of panels are available:
•
Traditional panels provide controls on a single window with minimal graphics.
•
System panels provide a more graphical interface than the traditional style and include more controls.
You can choose either style of panel, depending on your personal preference. 4. Open a panel for your system configuration by double-clicking its name in the list. For example, if your system includes an ICS-2000 and an AS50 autosampler, double-click either ICS-2000_Traditional_System_AS50.pan or ICS-2000_System_AS50.pan. 5. The Control panel opens, unconnected (see Figure 3-5). To connect to the timebase, open the Control menu and click the name of the ICS-2000 timebase in the list at the bottom of the menu.
Figure 3-5. ICS-2000 System Control Panel (Unconnected)
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Figure 3-6 shows a connected Control panel for an ICS-2000 system.
Figure 3-6. ICS-2000 System Control Panel (Connected)
3.4
Set Up the Eluent Reservoir 3.4.1
Filter the Deionized Water Filtering removes small particulates in the deionized water that may contaminate the pump check valves and cause erratic flow rates or loss of prime. An end-line filter (P/N 045987) is provided in the ICS-2000 Ship Kit (P/N 064375) for this purpose. Install the end-line filter on the end of the deionized water line, inside the reservoir. Verify that the end of the filter extends to the bottom of the reservoir and that the filter is submerged in deionized water. This prevents air from being drawn through the lines.
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3.4.2
Fill the Reservoir Fill the reservoir with ASTM filtered, Type I (18-megohm) deionized water.
3.4.3
Set the Eluent Level After filling the reservoir, enter the volume of liquid in the reservoir in one of the following locations:
• •
On the HOME page in the Eluent Level field (see Figure 3-7) In the Eluent Bottle field on the Chromeleon Control panel (see Figure 3-8)
The ICS-2000 determines the eluent usage by monitoring the flow rate and the length of time the pump is on. The ICS-2000 updates the field as the eluent is used up. A warning first appears if the level falls below 200 mL. Warnings are repeated at 100 mL and 0 mL. In order for the eluent level displayed on the screen to be accurate, the level must be entered by the user when the reservoir is filled. The ICS-2000 does not automatically detect when the reservoir is filled, nor when it is empty.
Enter the volume of liquid in the reservoir
Note: The Eluent Level field is updated as the liquid is used up.
Figure 3-7. Home Page: Setting the Eluent Level
Enter the volume of liquid in the reservoir
Note: The Eluent Bottle field and slider gauge are updated as the liquid is used up.
Figure 3-8. Chromeleon Control Panel: Setting the Eluent Level
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The STATUS page (see Figure 3-9) also displays the amount of liquid remaining in the reservoir and an estimate of how many hours remain before the eluent reservoir is empty. See Section C.6 for details about the STATUS PAGE.
Figure 3-9. Status Page
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3.4.4
Connect the Reservoir If it is not already connected, connect the ELUENT BOTTLE OUT line from the reservoir cap to the ELUENT IN line, which extends from the plumbing and cable chase on the top of the ICS-2000 (see Figure 3-10).
ELUENT BOTTLE OUT
ELUENT IN
Figure 3-10. Reservoir Connections
3.5
Check All Connections 1. Make sure the eluent reservoir is filled and the tubing connecting the reservoir to the ICS-2000 tubing is securely connected (see Figure 3-10). 2. Make sure the blue eluent generator electrical cable is connected to the EGC-1 (or EGC-2) connector. 3. If a CR-TC is installed, make sure the black CR-TC electrical cable is connected to the CR-TC connector. 4. If an EPM is installed, make sure the EPM electrical cable is connected to the EGC-2 (or EGC-1) connector. 5. Make sure the USB cable from the computer is connected to the USB receptacle on the ICS-2000 rear panel.
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3.6
Prime the Pump If you changed eluent or if the eluent lines are dry, prime the lines first with a syringe before following the procedure below to prime the pump. See Section B.13 for instructions on priming the lines with a syringe.
1. Verify that the priming valve on the primary pump head (see Figure 3-11) is closed (turned all the way clockwise). 2. Open the waste valve on the secondary pump head by turning the knob onequarter to one-half turn counterclockwise. Opening the valve directs the eluent flow path to waste and eliminates backpressure.
Secondary Pump Head
Waste Valve (open)
Priming Valve (close)
Primary Pump Head
Figure 3-11. Priming the Pump
3. Press Prime on the Chromeleon Control panel or the ICS-2000 touch screen HOME page. Confirm that the waste valve is open by pressing OK when the reminder message appears. The pump will begin pumping at approximately 3 mL/min. 4. Continue priming the ICS-2000 until all air and previous eluent are purged and no air bubbles are exiting the waste line. 5. Press Pump Off. 6. Close the waste valve. Do not overtighten. The pump is now ready for operation.
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3.7
Set System Operating Conditions NOTE This section is an overview of the steps needed to start up the system and begin running samples. Actual operating parameters (flow rate, cell heater temperature, suppressor current, etc.) depend on the application to be run. Refer to the column manual for the required parameters for your application.
Set or verify system operating parameters from either the Chromeleon Control panel or from the touch screen HOME page. Operating parameters can also be set automatically by loading a Chromeleon sequence. NOTE Clicking the System Startup button on the Chromeleon Control panel starts the pump, suppressor, eluent generator, and CR-TC. The flow rate, suppressor current, and eluent concentration settings that were in effect when the system was shut down are restored.
1. Verify that the pump is on and set to the correct flow rate. 2. Verify that the suppressor current is on and that the setting is correct. 3. Verify that the eluent generator is turned on and the correct concentration is set. Verify that the CR-TC (if installed) is turned on. Verify that the EPM (if installed) is on and the correct concentration is set. 4. Verify that the cell heater is set to the correct value. 5. Verify that the column heater is set to the correct value. Automatically Turning on the Suppressor and Eluent Generator
You can set up the ICS-2000 to turn on the suppressor, eluent generator, and CR-TC automatically when the pump is turned on. To do this:
• •
For the suppressor, select the Automatically turn on with pump option from the SUPPRESSOR page. For the eluent generator and CR-TC, select the option from the ELUENT page.
GENERATOR
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NOTE The suppressor, eluent generator, and CR-TC are always turned off automatically when the pump is turned off.
3.8
Equilibrate the System and Verify Operational Status NOTE You can monitor system functions (conductivity, pressure, cell temperature, etc.) from the Chromeleon Control panel or from the touch screen HOME page.
1. Allow the system to equilibrate. During equilibration, the Chromeleon Control panel displays the background conductivity (the conductivity of the eluent before sample injection) and the system backpressure. 2. Monitor the background conductivity. Refer to the column manual for the appropriate background conductivity for your application. 3. Offset the background and zero the reading by clicking the Autozero button on the Chromeleon Control panel (see Figure 3-4). 4. Monitor the system pressure from the Control panel to make sure it is at the expected pressure for the installed column (refer to the column manual for details) and is stable.
• • •
If the pressure is less than the expected amount, gas may be trapped in the system. To release the gas, remove the pump fitting on the injection valve port, labeled P (2). Allow the air to escape and then reconnect the fitting. If the pressure fluctuates by more than about 0.13 MPa (20 psi), prime the pump. See Section 4.3 for additional troubleshooting information. If the pressure is too high, there may be a restriction in the system plumbing (see Section 3.6). See Section 4.7 for troubleshooting information.
5. Verify that the baseline conductivity is at the expected reading for your application and is stable. In general, it should be Acquisition Off when sample data is collected. NOTE Data from Chromeleon manual processing is saved in the MANUAL sequence folder under the local datasource. This data is overwritten each time a new manual sample is processed. To save the data from a manual run, select the MANUAL folder, select File>Save As, and enter a new name for the sequence.
7. If you are controlling the ICS-2000 from the touch screens, select the PLOT button on the HOME page to view a plot of the conductivity data.
3.11.2 Automatic (Batch) Sample Processing For batch processing, you use Chromeleon to create a list of samples (a sequence) to be processed automatically. For each sample, the sequence includes a program with commands and parameters for controlling the ICS-2000, controlling the autosampler (if used), and acquiring sample data. The sequence also includes a quantification method for peak identification and area determination. Additional sample processing parameters are included in the sequence (for example, the sample name, sample type, injection volume, etc.). After defining the sequence, you can start batch processing.
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ICS-2000 Ion Chromatography System
1. Complete the steps in Sections 3.2 through 3.8 to prepare for operation and to start up the ICS-2000. 2. Create a new sequence or modify an existing one. To create a new sequence: a. In the Browser, select File>New. Select Sequence (using Wizard) and click OK. b. Complete the steps in the Sequence Wizard, adding the desired number of samples and standards to the list. For help with any of the steps, click the Help button on the Sequence Wizard page. NOTE A simple way to get started is to select the “Use Application Template” option in Step 4 of the Sequence Wizard. This option lets you select a column and suppressor type from a list of applications. The Wizard then copies a program and quantification method, appropriate for the selected application, to the sequence folder and adds them to the sequence definition.
3. To start the sample processing, make sure the System Control panel is open (see Section 3.3) and is the active window. Then, select Batch>Edit. The Batch dialog box opens (see Figure 3-13).
Figure 3-13. Batch Dialog Box
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4. Click the Add button on the Batch List tab and add the sequence you created in Step 2. See Figure 3-14 for an example.
Figure 3-14. Batch Dialog Box with an Example Sequence Added to the Batch List
5. To start the batch, click Start.
3.12 Maintenance This section describes routine maintenance procedures that users may perform. All other maintenance procedures must be performed by Dionex personnel. As Needed
•
Regularly check the eluent reservoir and refill when needed.
Daily
• •
Check the ICS-2000 component mounting panel (see Figure 2-8) for leaks or spills. Wipe up spills. Isolate and repair leaks (see Section 4.2). Rinse off any dried eluent with deionized water. Check the waste container daily and empty when needed.
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ICS-2000 Ion Chromatography System
Weekly
• •
•
Once a week, check fluid lines for crimping or discoloration. Relocate any pinched lines. Replace damaged lines. Check the junctions between the pump heads and the pump casting for evidence of liquid leaks. If the piston seal wash tubing is not connected, check the drain tubes at the rear of the pump heads for evidence of moisture. Normal friction and wear may gradually result in small liquid leaks around the piston seal. If unchecked, these leaks can gradually contaminate the piston housing, causing the pump to operate poorly. If leaks occur, replace the piston seals (see Section 5.6). Check the end-line filter (P/N 045987) and change if needed. When new, endline filters are pure white. If the system is in continuous operation, change the end-line filter weekly, or whenever it becomes discolored. Replace the filter more often if bacterial buildup is visible or if the eluent does not contain solvent. NOTE It is especially important to regularly replace end-line filters when using aqueous eluents, which may contaminate the filter with bacteria or algae. The bacterial buildup may not be visible.
Every Six Months
•
Calibrate the cell (see Section 5.1.3).
•
Calibrate the vacuum degas assembly (see Section 5.1.5).
•
Replace the pump piston rinse seals and piston seals (see Section 5.6).
Yearly
• •
•
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Rebuild the injection valve (see Section 5.4). Replace the AS40 Automated Sampler tip and tubing. The AS40/ASM Maintenance Kit (P/N 055647) contains all of the components required to replace the sampling tip and the tubing between the tip and the injection valve. Instructions are included with the kit. Perform the AS or AS50 (USB) preventive maintenance procedure. The AS or AS50 (USB) Maintenance Kit (P/N 060581) contains all of the required components and instructions for performing the procedure.
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4 • Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the ICS-2000. Turn to the section of this chapter that best describes the operating problem or symptom that has been observed. Each section lists possible causes of the problem or symptom in order of probability. A systematic troubleshooting approach is the most effective way to determine the root cause. If you are unable to resolve a problem by following the instructions here, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office. Please have this chapter at hand when talking with Technical Support personnel.
4.3
Error Messages The Moduleware (the instrument control firmware installed in each ICS-2000 module) periodically checks the status of certain parameters. If a problem is detected, it is displayed on the touch screen. Error messages are also reported to Chromeleon and logged in the Audit Trail. Each error message is preceded by an icon that identifies the seriousness of the underlying problem (see the table below). You can change the severity level assigned to a problem whenever appropriate. Icon
Severity Level
Description
Warning
A message is displayed in the Audit Trail, but the current run is not interrupted.
Error
A message is displayed in the Audit Trail, and the system attempts to correct the problem (sometimes by using an alternative parameter). An Error never interrupts the current analysis; however, if it occurs during the Ready Check, the analysis will not be started. A message is displayed in the Audit Trail, and the running batch is aborted.
Abort
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The table below lists the most frequently observed ICS-2000 error messages. For troubleshooting assistance, refer to the page indicated in the table. Alarms and Error Conditions
See
Column heater exceeds safe temperature
page 3
Column heater open circuit
page 3
Column heater short circuit
page 4
CR-TC over current error
page 4
CR-TC stopped for zero flow rate
page 4
Degas calibration failed
page 4
EGC board not present
page 5
EGC-1 calibration error
page 5
EGC-1 disconnected error
page 5
EGC-1 invalid concentration vs flow rate error
page 6
EGC-1 invalid flow rate error
page 6
EGC-1 over current
page 7
EGC-1 over voltage
page 7
EGC-2 calibration error
page 5
EGC-2 disconnected error
page 5
EGC-2 invalid concentration vs. flow rate error
page 6
EGC-2 invalid flow rate error
page 6
EGC-2 over current
page 7
EGC-2 over voltage
page 7
Hardware not present
page 7
Leak sensor wet
page 7
Load/inject valve error
page 8
Option not installed
page 8
Pressure slope calibration error
page 9
Pump motor lost control
page 9
Pump pressure hardware error
page 9
Pump over pressure
page 9
Pump under pressure
page 10
Table 4-4. ICS-2000 Alarms and Error Messages Summary
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Alarms and Error Conditions
See
Suppressor over current
page 10
Suppressor over voltage
page 11
Suppressor over power
page 11
Suppressor not connected
page 11
Suppressor stopped for flow rate
page 12
Table 4-4. ICS-2000 Alarms and Error Messages Summary (Continued)
4.1
Troubleshooting Error Messages
COLUMN HEATER EXCEEDS SAFE TEMPERATURE This error occurs when the column heater temperature is higher than the maximum allowed. This error may occur if the ICS-2000 is operating in an extreme environment (greater than 40 °C (104 °F)). To troubleshoot: Refer to Section A.3 for environmental specifications.
COLUMN HEATER OPEN CIRCUIT This error occurs when the column heater is unplugged from the component panel. To troubleshoot: 1. Check that the column heater is plugged into the component panel. 2. If the error persists, the column heater may be faulty. Replace the column heater (see Section 5.11).
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COLUMN HEATER SHORT CIRCUIT This error occurs when there is a short circuit on the thermistor input used to measure the column heater temperature. This error indicates a faulty column heater. To troubleshoot: Replace the column heater (see Section 5.11).
CR-TC OVER CURRENT ERROR This error occurs when the current applied to the CR-TC exceeds the maximum current allowed. To troubleshoot: 1. Check the CR-TC cable connection. 2. If the error persists, contact Dionex for assistance. There may be a malfunction in the CR-TC control electronics.
CR-TC STOPPED FOR ZERO FLOW RATE This message appears when you click the Shutdown button on the Chromeleon Control panel. The message also appears when you turn off the pump flow while the EGC current (and CR-TC) is on. The CR-TC is automatically turned off. To troubleshoot: If the pump stopped unexpectedly, see Section 4.5 for pump troubleshooting information.
DEGAS CALIBRATION FAILED This error occurs when the degas vacuum does not reach the expected level during calibration.
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To troubleshoot: 1. Retry the calibration. 2. If calibration still fails, the vacuum degas assembly may need to be replaced. Contact Dionex for assistance.
EGC BOARD NOT PRESENT This error occurs if Chromeleon sends a command to the ICS-2000 related to the eluent generator, but the eluent generator controller board is either not installed or the ICS-2000 does not recognize the installed board. To troubleshoot: Contact Dionex for assistance. The ICS-2000 electronics components cannot be serviced by the user.
EGC-1 CALIBRATION ERROR EGC-2 CALIBRATION ERROR This error occurs if the measured current is outside the expected range when running the eluent generator calibration procedure. To troubleshoot:
• •
Review the procedure to verify that you set up the ICS-2000 correctly and then rerun the calibration. If the error message reappears, contact Dionex for assistance.
EGC-1 DISCONNECTED ERROR EGC-2 DISCONNECTED ERROR This error occurs if Chromeleon sends a command to set an eluent generator parameter when the EGC is disconnected. The error also can occur if you attempt to run the EGC verification test when the EGC is disconnected.
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To troubleshoot: 1. Verify that the eluent generator cartridge is connected to the EGC-1 connector on top of the ICS-2000 (see Figure 2-7). 2. If the error persists, contact Dionex for assistance. There may be a malfunction in the EGC control electronics.
EGC-1 INVALID CONCENTRATION VS. FLOW RATE ERROR EGC-2 INVALID CONCENTRATION VS. FLOW RATE ERROR The maximum eluent concentration that can be set for a particular application depends on the suppressor type, the EGC type, and the flow rate. This error occurs if the selected concentration is too high for the current flow rate. To troubleshoot: Refer to the column manual, which is included on the Dionex Reference Library CD-ROM (P/N 053891), for the concentration of eluent to use with your application. Reset the eluent concentration and/or the flow rate to the recommended values.
EGC-1 INVALID FLOW RATE ERROR EGC-2 INVALID FLOW RATE ERROR This error occurs if the flow rate is set to a value not supported by the eluent generator. The ICS-2000 allows a flow rate range of 0.00 to 5.00 mL/min without an eluent generator. With an eluent generator, the allowed range is 0.10 to 3.00 mL/min.The recommended operating range is 0.40 to 2.00 mL/min. To troubleshoot: Set the flow rate to a value within the allowed range.
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EGC-1 OVER-CURRENT EGC-2 OVER-CURRENT This error occurs when the current applied to the eluent generator cartridge exceeds the maximum current allowed. Under these conditions, the EGC current is turned off to prevent damage to the EGC. This error may occur if the liquid flow to the cartridge is interrupted. To troubleshoot:
•
See Section 4.5 for troubleshooting when there is no flow from the pump.
EGC-1 OVER-VOLTAGE EGC-2 OVER-VOLTAGE This error occurs when the current applied to the eluent generator cartridge exceeds the maximum current allowed. The EGC current is turned off to prevent damage to the EGC. This error may occur if the liquid flow to the cartridge is interrupted. To troubleshoot:
•
See Section 4.5 for troubleshooting when there is no flow from the pump.
HARDWARE NOT PRESENT This error indicates a problem in the ICS-2000 electronics. To troubleshoot:
•
Contact Dionex for assistance. The ICS-2000 electronics components cannot be serviced by the user.
LEAK SENSOR WET The leak sensor is installed in the drip tray at the bottom of the component panel (see Figure 2-8). If liquid accumulates in the tray, the sensor signals the problem and the “Leak sensor wet” error message appears.
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To troubleshoot: 1. Locate the source of the leak by visually inspecting the tubing, fittings, and components on the component panel. 2. Tighten fittings or replace tubing and fittings as required. Refer to Section 4.2 for detailed troubleshooting of various types of leaks. 3. After fixing the leak, dry the drip tray thoroughly to prevent the leak sensor from triggering additional error messages.
LOAD/INJECT VALVE ERROR If the injection valve fails to switch position within 1 second of being toggled, the ICS-2000 Moduleware reports an error to Chromeleon and the “Load/Inject valve error” message appears. To troubleshoot: 1. If a sequence is being executed, terminate the sequence by selecting Batch>Stop on the Chromeleon menu. 2. Turn off the ICS-2000 power briefly and then restart. 3. Try to toggle the valve from Load to Inject by clicking the Load and Inject buttons on the ICS-2000 Control panel in Chromeleon or on the touch screen HOME page. 4. If the problem persists, contact Dionex for assistance.
OPTION NOT INSTALLED This error occurs if a command is issued to control an option that is not installed. To troubleshoot:
•
4-8
Check the Chromeleon Server Configuration program to verify that the option is enabled.
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PRESSURE SLOPE CALIBRATION ERROR This error occurs if you try to calibrate the pressure slope when the pressure is less than 3 MPa (500 psi). To troubleshoot:
•
Contact Dionex for assistance.
PUMP MOTOR LOST CONTROL This error indicates a problem in the pump controller electronics. To troubleshoot:
•
Contact Dionex for assistance. The ICS-2000 electronics components cannot be serviced by the user.
PUMP PRESSURE HARDWARE ERROR This error indicates a problem in the pump controller electronics. To troubleshoot:
•
Contact Dionex for assistance. The ICS-2000 electronics components cannot be serviced by the user.
PUMP OVER PRESSURE If the system pressure exceeds the set limit for at least 0.5 seconds, this error message appears and the pump stops. Pressure limits can be set in the Chromeleon Server Configuration or in the control program. The limits can also be set on the touch screen PUMP page (see Section C.7.1). To troubleshoot: 1. Check for blockages in the liquid lines by working your way backward from the cell to the pump. See Figure 2-13 for the system flow schematic. 2. Check that the flow rate is set to the correct value.
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3. Check that the high pressure limit is set to the correct value. 4. Restart the pump.
PUMP UNDER PRESSURE If the system pressure falls below the low pressure limit, the pump stops and this error message appears. Pressure limits can be set in the Chromeleon Server Configuration or in the control program. The limits can also be set on the touch screen PUMP page (see Section C.7.1). To troubleshoot: 1. Make sure the eluent reservoir is full. 2. Check for liquid leaks (see Section 4.2). 3. Check that the waste valve is closed. 4. Prime the pump (see Section B.13). 5. Restart the pump.
SUPPRESSOR OVER CURRENT This error may be caused by an expended or dirty suppressor or by a malfunction in the suppressor controller electronics. To troubleshoot: 1. Follow the instructions in the suppressor manual to regenerate the suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). 2. Follow the instructions in the suppressor manual to clean the suppressor. 3. If a malfunction in the suppressor controller is suspected, contact Dionex for assistance. The ICS-2000 electronics components cannot be serviced by the user.
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4 • Troubleshooting
SUPPRESSOR OVER VOLTAGE This error occurs if you turn on the suppressor but the ICS-2000 cannot establish a connection with the suppressor. To troubleshoot: 1. Check the suppressor cable connection (see Section 5.10). 2. If the error persists, replace the suppressor (see Section 5.10).
SUPPRESSOR OVER POWER This error occurs when, in order to maintain the selected current, the ICS2000 is required to apply a higher voltage than the suppressor can support. To troubleshoot:
• • •
Reduce the flow rate. Rehydrate the suppressor. Refer to the suppressor manual for instructions. Suppressor manuals are included on the Dionex Reference Library CDROM (P/N 053891). If the error persists, replace the suppressor (see Section 5.10).
SUPPRESSOR NOT CONNECTED This error occurs if you turn on the suppressor and the ICS-2000 cannot establish a connection with the suppressor. To troubleshoot: 1. Check the suppressor cable connection (see Section 5.10). 2. If the error persists, contact Dionex for assistance. There may be a problem in the suppressor controller electronics. The ICS-2000 electronics components cannot be serviced by the user.
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ICS-2000 Ion Chromatography System
SUPPRESSOR STOPPED FOR ZERO FLOW RATE This error message appears when you click the Shutdown button on the Chromeleon Control panel. The message also appears anytime you turn off the pump flow while the suppressor is on. The suppressor is automatically turned off to prevent damage to the suppressor. To troubleshoot:
•
4.2
If the pump stopped unexpectedly, see Section 4.5 for pump troubleshooting information.
Liquid Leaks •
Leaking fitting Locate the source of the leak. Tighten or, if necessary, replace the liquid line connection (see Section 5.3). Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891).
•
Broken liquid line Replace the line and fittings with the same length and internal diameter tubing (see Section 5.3).
•
Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked. Also, if the blocked line is a waste line, make sure it is not elevated at any point after it exits the ICS-2000. If a line is blocked, replace it (see Section 5.3).
•
Loose pump check valve 1. Make sure the check valves are firmly seated in the pump head. If they are not, tighten them carefully with an open-end wrench just until the leak stops. 2. If the leak persists, replace the check valve (see Section 5.5).
•
Leaking seal wash port Leaking from the seal wash port indicates a leaking piston seal. Replace the seal (see Section 5.6).
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4 • Troubleshooting •
Damaged pump piston seal 1. Replace the piston seal (see Section 5.6). 2. If the leak persists, replace the piston (see Section 5.7).
•
Pump head not tight against casting Carefully tighten the pump head mounting nuts just until the leak stops. DO NOT OVERTIGHTEN!
•
Leaking pressure transducer 1. Make sure the liquid line connections into the pressure transducer are tight. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891). Replace any damaged fittings. 2. If the pressure transducer continues to leak, contact Dionex for assistance.The pressure transducer cannot be serviced by the user.
•
Leaking pump head waste valve Make sure the waste valve is closed. To close the valve, turn the knob clockwise, and tighten fingertight. DO NOT OVERTIGHTEN! Overtightening may damage the valve and the pump head. If the leak persists, replace the waste valve O-ring (see Section 5.8).
•
Leaking suppressor Refer to the suppressor manual for troubleshooting procedures. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).
•
Leaking injection valve 1. Make sure the liquid line connections to the transducer are tight. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891). Replace any damaged fittings. 2. Liquid leaks from behind the valve stator may indicate a scratched rotor seal. Rebuild the injection valve (see Section 5.4).
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ICS-2000 Ion Chromatography System •
Leaking cell 1. Check the waste lines for blockage; trapped particles can plug the lines and cause a restriction and/or leak. If necessary, clear the waste lines by reversing the direction of flow. 2. Make sure the plumbing downstream from the cell is clear; a blockage may overpressurize the cell, causing it to leak. If the problem continues, contact Dionex for assistance.
4.3
Pump Difficult to Prime or Loses Prime Excessive pressure fluctuations (more than 3% difference from one pressure reading to the next) indicate that the pump is out of prime.
•
Empty eluent reservoir and/or no eluent connected Fill the reservoir. Make sure all connections are secure.
•
Eluent improperly or insufficiently degassed Check the vacuum degas settings: 1. Open the Chromeleon Server Configuration program, select the ICS-2000 device icon under the timebase, and select Edit>Properties (or doubleclick the ICS-2000 device icon).
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4 • Troubleshooting
2. Select the Options tab (see Figure 4-1).
Figure 4-1. ICS-2000 Server Configuration Properties: Options
3. Under Installed Options, verify that the Degas check box is selected. 4. Check the Degas Mode settings. Select either the Monitor option or the Cycle option. If you select Cycle, set the time On to 30 seconds and the time Off to 10 minutes. If Cycle is already selected, try increasing the time on or decreasing the time off. NOTE Degas Mode options can also be selected from the touch screen PUMP page (see Section C.7).
•
End-line filter is dirty or clogged When new, end-line filters (P/N 045987) are pure white. If the system is in continuous operation, change the end-line filter weekly, or whenever it becomes discolored. Replace the filter more often if bacterial buildup is visible or if the eluent does not contain solvent.
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ICS-2000 Ion Chromatography System
NOTE It is especially important to regularly replace end-line filters when using aqueous eluents, which may contaminate the filter with bacteria or algae. The bacterial buildup may not be visible.
•
Blockages in inlet tubing Kinked or clogged tubing causes the pump to be “starved” for eluent. Replace the tubing and fittings (see Section 5.3).
•
Dirty check valve Clean or replace the pump check valve (see Section 5.5).
•
Liquid leaks at junction between pump head and pump casting Use the open-end wrench (P/N 014605) provided in the ICS-2000 Ship Kit (P/N 057905) to tighten the two acorn nuts that attach the pump head to the pump housing (see Figure 5-11). Tighten the nuts evenly (12 in-lb torque). If the leak persists, replace the piston seal (see Section 5.6).
•
Liquid leaks from the seal wash port Replace the piston seal (see Section 5.6).
•
Scratched pump piston Check the pump pistons for scratches and replace if necessary (see Section 5.7).
4.4
Pump Does Not Start •
No power (front Power LED indicator is not lit) Check that the power cord is plugged in. Check the main power fuses and replace if needed (see Section 5.16).
•
No communication between ICS-2000 and Chromeleon Verify that the USB cable is connected correctly. See Section B.5 for installation instructions.
•
Pump is turned off Turn on the pump from either the Chromeleon Control panel or the ICS-2000 touch screen HOME page.
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4 • Troubleshooting •
Flow rate is set to 0 Set the flow rate from either the Chromeleon Control panel or the ICS-2000 touch screen HOME page.
4.5
No Flow •
Pump waste or priming valve open (see Figure 4-2). Close the valves by turning the knobs clockwise until fingertight. DO NOT OVERTIGHTEN! Overtightening may damage the valve and the pump head.
Priming Valve Waste Valve
Figure 4-2. Waste and Priming Valves
•
Flow rate is set to 0 Set the flow rate from the Chromeleon Control panel or from the touch screen HOME page.
•
Eluent valve is closed Open the eluent valve from the Chromeleon Control panel or from the touch screen PUMP page.
•
Pump not primed Prime the pump (see Section B.13).
•
Broken pump piston Replace the piston (see Section 5.7).
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ICS-2000 Ion Chromatography System •
Eluent generator degas tubing assembly ruptured Replace the EluGen cartridge holder (see Section 5.17).
4.6
Erratic Flow/Pressure Reading •
Pump needs priming Prime the pump (see Section B.13).
•
Damaged piston seal Replace the piston seal (see Section 5.6).
•
Dirty pump check valve Clean or replace the check valve (see Section 5.5).
•
Leaking liquid lines or fittings Check the liquid lines and fittings for small leaks. Tighten or, if necessary, replace the liquid line connection (see Section 5.3). Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891).
4.7
Excessive System Backpressure •
Restriction in the system plumbing Check all liquid lines for crimping or blockage. Make sure the ferrule fittings are not overtightened onto tubing. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for details. The manual is on the Dionex Reference Library CD-ROM (P/N 053891). If you have trouble isolating the restriction, refer to Section 5.2.
•
Plugged or damaged fitting Isolate the faulty fitting by loosening fittings one by one until the pressure returns to normal. Repair or replace the fitting (see Section 5.3).
•
Flow rate through the columns too high Set the correct rate for your application. If an incorrect flow rate calibration is suspected, calibrate the flow (see Section 5.1.4).
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4 • Troubleshooting •
Clogged column bed supports Refer to the instructions in the column manual for troubleshooting guidance. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).
•
Contaminated columns Clean the columns as instructed in the column manual.
•
Plugged injection valve passages Rebuild the injection valve (see Section 5.4).
4.8
Peak “Ghosting” “Ghosting” is the appearance of extraneous peaks in a chromatogram. These may be late-eluting peaks from a previous injection, or they may be the result of a contaminated standard or eluent, or a malfunctioning injection valve. These peaks may co-elute with peaks of interest, resulting in nonreproducible peak heights/areas.
•
Insufficient time between sample injections Wait until the previous sample has been completely eluted before making another injection.
•
Insufficient flush between samples Flush the sample loop with at least 10 loop volumes of deionized water or sample between sample injections.
•
Incorrect or contaminated standards Remake standards.
•
Incorrect or contaminated eluent Verify that the correct eluent concentration is selected. Install or replace the end-line filter on the end of the deionized water line (see Section 3.4.1).
•
Malfunctioning injection valve 1. Rebuild the injection valve (see Section 5.4). 2. If the valve leak persists, contact Dionex for assistance.
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ICS-2000 Ion Chromatography System
4.9
Nonreproducible Peak Height or Retention Time •
Column overloading Dilute the sample (see Section 3.9).
•
Liquid leaks Locate and eliminate the leaks (see Section 4.2).
•
Incomplete or imprecise filling of the sample loop 1. Fill the sample loop until excess sample exits the waste line. 2. Inspect the 1-cc syringe (P/N 016388) and replace if damaged.
•
Pump not primed properly Prime the pump (see Section B.13).
4.10 Abnormal Retention Time or Selectivity •
Incorrect eluent Check the EGC concentration setting.
•
Contaminated or degraded sample Take appropriate precautions when preparing and storing samples to prevent contamination and degradation (see Section 3.9).
•
Contaminated column 1. Clean the column as instructed in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). 2. If cleaning is unsuccessful, replace the column.
4.11 No Cell Response •
Cell not properly installed Verify that the cell front cover is flush against the component panel. If necessary, tighten the two mounting screws. When the cell is correctly installed and the screws tightened, an electronics connector on the cell plugs into a receptacle inside the ICS-2000.
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4 • Troubleshooting •
No flow from pump This condition has several possible causes. See Section 4.4 and Section 4.5 for details.
•
Cell electronics malfunctioning Use the Chromeleon Wellness Panel diagnostics to test the electronics (see Section 5.1 and the Chromeleon online Help for instructions). If the variance reading is outside the tolerance range (less than 1 µS), the electronics are malfunctioning. Contact Dionex for assistance. The ICS-2000 electronics cannot be serviced by the user.
4.12 High Cell Output •
Background not suppressed by suppressor Verify that the suppressor is turned on and the current is set to the correct value. Refer to the suppressor manual for additional troubleshooting guidance. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).
•
Sample concentration too high Dilute the sample Section 3.9.3.
•
Wrong eluent Check that you are using the correct eluent for your application.
•
Background conductivity not offset from conductivity reading Before making an injection, allow the background conductivity to equilibrate, and then press Autozero on the Chromeleon Control panel or the ICS-2000 touch screen HOME page.
•
Cell out of calibration Recalibrate the cell (see Section 5.1.3).
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ICS-2000 Ion Chromatography System
4.13 Baseline Noise or Drift •
Flow system leak; erratic baseline Check all fittings and liquid lines for leaks. Tighten or, if necessary, replace all liquid line connections. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891).
•
Trapped gases Release any trapped gases in the cell by loosening the lines to and from the cell and then retightening them. Also loosen and retighten the fittings to and from the suppressor eluent ports.
•
Pump not properly primed Prime the pump (see Section B.13).
•
Incorrect eluent Check the EGC concentration setting.
•
Inadequate system backpressure Add backpressure tubing between the injection valve and the ELUENT OUT port on the EGC to maintain a pressure of 16 ± 0.7 MPa (2300 ± 100 psi). See Section B.16.1 for details.
•
Rapid changes in ambient temperature Make sure the ambient temperature is between 4 and 40 °C (40 and 104 °F). Make sure air conditioning and heating vents are directed away from the ICS2000 and the ICS-2000 front door is closed.
•
Insufficient system equilibration following changes to operating parameters; especially apparent when operating at high sensitivities Allow a longer system equilibration time (up to 2 hours) before starting operation.
•
Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).
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4 • Troubleshooting •
Cell above or below temperature Contact Dionex for assistance.
•
Damaged piston seal Replace the piston seal (see Section 5.6).
4.14 Vacuum Degas Assembly Does Not Run •
Degas option not enabled in Chromeleon 1. Open the Chromeleon Server Configuration program. Select the ICS2000 device icon under the timebase and select Edit>Properties (or double-click the ICS-2000 device icon). Select the Options tab (see Figure 4-3).
Figure 4-3. ICS-2000 Server Configuration Properties: Options.
2. Under Installed Options, verify that the Degas check box is selected.
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ICS-2000 Ion Chromatography System
3. Under Degas Mode, verify that the Always Off option is not selected. If it is, select one of the following settings:
•
Cycle, and select On: 30 seconds and Off: 10 minutes
•
Monitor
4. If the Degas Mode settings are correct, but the degas assembly still does not run, test the assembly by selecting the Always On option. The pump should turn on immediately. If it does not, the vacuum degas assembly may need to be replaced. Contact Dionex for assistance. NOTE Degas Mode options can also be selected from the touch screen PUMP page (see Section C.7). Select the Degas Mode, Always On option only when testing the vacuum degas assembly. Do not select the Always On option for routine use.
5. If the degas pump runs when you select Always On, but does not run when Monitor mode is selected, recalibrate the degas assembly (see Section 5.1.5).
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5 • Service This chapter describes ICS-2000 service and repair procedures that the user can perform. All procedures not included here, including electronics-related repair procedures, must be performed by Dionex personnel. For assistance, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office. Before replacing any part, refer to the troubleshooting information in Chapter 4 to isolate the cause of the problem. Substituting non-Dionex parts may impair performance, thereby voiding the product warranty. Refer to the warranty statement in the Dionex Terms and Conditions for more information.
5.1
Diagnostic and Calibration Procedures Diagnostic and calibration procedures can be performed either from the touch screen or from the Chromeleon Wellness Panel (see Figure 5-1). For an overview of the Wellness Panel features, see Section 5.1.1. For an overview of the diagnostic and calibration touch screen, see Section 5.1.2. For instructions on performing calibration and diagnostic procedures, see the following sections:
•
Calibrating the Conductivity Cell (Section 5.1.3)
•
Calibrating the Flow Rate (Section 5.1.4)
•
Calibrating the Vacuum Degas Assembly (Section 5.1.5)
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ICS-2000 Ion Chromatography System
5.1.1
Chromeleon Wellness Panel Overview NOTE Do not open a System Wellness Control panel if the name includes “Service.pan.” These Wellness panels are reserved for use by Dionex Service Representatives. To Open the Wellness Panel
1. Open the Chromeleon Browser and expand the Dionex Templates folder. 2. Expand the Panels folder and then the Wellness folder. 3. In the right pane of the Browser window, double-click ICS1000_1500_2000_Wellness_user.pan. The Wellness Panel appears. 4. Open the Control menu and click the name of the ICS-2000 timebase at the bottom of the menu. This connects the Wellness Panel to the ICS-2000 and enables the controls on the panel.
Figure 5-1. Chromeleon Wellness Panel
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5 • Service
Use the Wellness Panel to perform the following functions:
•
Calibrate the pump flow rate
•
Calibrate the vacuum degas assembly
•
Calibrate the conductivity cell
•
Test the conductivity cell electronics, using a dummy cell
•
Upload calibration values from the ICS-2000 to the Chromeleon Wellness database
After completing a calibration procedure from the touch screen, always update the Chromeleon Wellness database by clicking the Upload button on the Chromeleon Wellness Panel (see Figure 5-1). This action ensures that the current calibration information is stored in Chromeleon as well as in the ICS-2000.
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ICS-2000 Ion Chromatography System
5.1.2
Diagnostic and Calibration Touch Screen Overview Select DIAGNOSTIC from the touch screen menu of pages. The DIAGNOSTIC page opens (see Figure 5-2). From there, you can access individual diagnostic and calibration pages. NOTE The Service button provides access to service functions that are performed only by Dionex personnel. An access code is required to go to the service pages.
Figure 5-2. System Diagnostic Menu Page NOTE The Diagnostic touch pages, EGC1 and EGC2 and EGC1 and EGC2 RESISTIVE LOAD VERIFICATION, display the results of the EluGen cartridge validation procedure, which is normally performed by Dionex personnel. Contact Dionex for more information.
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5 • Service
5.1.3
Calibrating the Conductivity Cell When to Calibrate
•
After every 6 months of use
NOTE Do not use this procedure to calibrate a new cell. If you are replacing a cell, see the instructions in Section 5.9 to install the new cell and calibrate it. Items Needed
Description
1.0 mM KCl solution
Prepare by dissolving 0.07456 g of reagentgrade KCl in 1 liter of 18-megohm DI water.
Backpressure tubing to provide at least 7 MPa (1000 psi)
Use 0.076-mm (0.003-in) ID yellow PEEK tubing (P/N 049715).
1. Open the ICS-2000 Wellness Panel in Chromeleon (see Section 5.1.1), or open the touch screen ELECTRIC CONDUCTIVITY CALIBRATION page (see Figure 5-3).
Figure 5-3. Electric Conductivity Calibration Page
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ICS-2000 Ion Chromatography System
2. On the Wellness Panel under Electric Conductivity Cell Calibration, click Offset Cal, or touch Run Offset Cal on the ICS2000 touch screen. 3. When the offset calibration is complete, click Slope Cal on the Wellness Panel, or touch Run Slope Cal on the ICS-2000 touch screen. 4. If you are using the Wellness Panel, click Log to record the new calibration values in the Audit Trail. 5. Disconnect the pump output line from the injection valve. 6. Disconnect the line from the suppressor ELUENT OUT port to the cell inlet and connect the pump output line directly to the cell inlet. 7. Verify that the backpressure is at least 7 MPa (1000 psi). 8. If you are using the touch screens to perform the calibration, open the CONDUCTIVITY CELL page (see Figure 5-4).
Figure 5-4. Conductivity Cell Page
9. On the Wellness Panel under Conductivity Cell Calibration, click Cell 35 C, or touch 35 C on the ICS-2000 touch screen. Allow the cell to reach this temperature and then wait an additional 5 minutes to let it stabilize. When the temperature has stabilized, “=” is displayed to the right of the temperature reading on the CONDUCTIVITY CELL page.
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5 • Service
10. Select 1.00 mL/min to begin pumping 1.00 mM KCl through the cell at 1.0 mL/min. 11. Wait until the total conductivity reading stabilizes (in about 15 minutes) and then select Calibrate on the Wellness Panel or the touch screen CONDUCTIVITY CELL page. After calibration, the conductivity reading should be 147.00 ± 2 µS and the cell constant should be between 120 and 180. If this is not the case, contact Dionex for help. 12. If you are using the Wellness Panel, click Log to record the new calibration values in the Audit Trail. 13. If you are using the ICS-2000 touch screen, record the new calibration values in the Chromeleon Wellness database. To do this, open the Wellness Panel (see Section 5.1.1) and click Upload under Update Wellness Database. 14. Flush the KCl solution from the system by pumping deionized water through the cell. When the conductivity drops to less than 1 µS/cm, stop the pump. 15. Reconnect the pump to the injection valve and reconnect the line from the suppressor to the cell inlet.
5.1.4
Calibrating the Flow Rate When to Calibrate
If you run the ICS-2000 Operational Qualification or Performance Qualification and it fails. Items Needed
•
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0.076-mm (0.003-in) ID yellow PEEK tubing (P/N 049715) to create 14 ± 2 MPa (2000 ± 300 psi) of backpressure (if needed)
•
High purity ASTM filtered, Type I (18 megohm-cm) deionized water
•
Balance capable of weighing more than 10 g with 0.001 g readability
•
Tared beaker
5-7
ICS-2000 Ion Chromatography System
To Calibrate
1. Open the ICS-2000 Wellness Panel in Chromeleon (see Section 5.1.1), or open the ICS-2000 touch screen FLOW RATE page (see Figure 5-5).
Figure 5-5. Flow Rate Page
2. Verify that there is 14 ± 1.4 MPa (2000 ± 200 psi) of backpressure. 3. On the Chromeleon Wellness Panel under Pump Flow Rate Calibration, select Reset Cal, or touch Reset Cal on the ICS-2000 touch screen. 4. Select 1 mL/min to set the flow rate and begin pumping deionized water. 5. Allow the pump to stabilize for 20 minutes. 6. If you are using the Wellness Panel, click 5.00 min to start the timer. If you are using the touch screen, start an external timer. Immediately start collecting water into the tared beaker. 7. Collect the water for exactly 5.00 minutes. 8. Enter the weight of the water (in grams). 9. If you are using the Wellness Panel, click Calibrate to download the value to the ICS-2000.
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5 • Service
10. To recheck the value, wait at least 15 minutes, and then repeat the calibration. 11. If you are using the Wellness panel, click Log to record the new calibration value in the Audit Trail. 12. If you performed the calibration from the ICS-2000 touch screen, record the new calibration values in the Chromeleon Wellness database. To do this, open the Wellness Panel (see Section 5.1.1) and click Upload.
5.1.5
Calibrating the Vacuum Degas Assembly When to Calibrate
•
After every 6 months of use
1. Open the ICS-2000 Wellness Panel in Chromeleon (see Section 5.1.1), or open the ICS-2000 touch screen PUMP DEGAS page (see Figure 5-6).
Figure 5-6. Pump Degas Page
2. On the Wellness Panel under Degas Calibration, select Calibrate, or touch Calibrate on the ICS-2000 touch screen. The degas pump runs for 90 seconds to allow a vacuum to be created. After 90 seconds, the
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ICS-2000 Ion Chromatography System
vacuum degas pressure reading is recorded. When the vacuum degas assembly is running in monitor mode, this calibration value is used to determine when to turn on the degas pump. 3. If you are using the Wellness panel, click Log to record the new calibration value in the Audit Trail. 4. If you performed the calibration from the ICS-2000 touch screen, record the new calibration values in the Chromeleon Wellness database. To do this, open the Wellness Panel (see Section 5.1.1) and click Upload under Update Wellness Database.
5.2
Isolating a Restriction in the Liquid Lines A restriction in the liquid plumbing will cause excessive system backpressure. 1. Begin pumping eluent through the system (including the columns). 2. Follow the ICS-2000 flow schematics in Figure 5-7, Figure 5-8, or Figure 5-9 and work backward through the system, beginning at the suppressor Regen Out port. One at a time, loosen each fitting and observe the pressure. The connection at which the pressure drops abnormally indicates the point of restriction. NOTE The numbers on the ICS-2000 flow schematic indicate the order in which liquid flows through the system components.
If the restriction has caused such high pressure that the system cannot be operated, you must work forward through the flow schematics, adding parts one at a time until an abnormal pressure increase (and hence, the restriction) is found. 3. If the restriction is in the tubing or fitting, remove the restriction by back flushing or by replacing the tubing or fitting (see Section 5.3).
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5 • Service
To the pump Degas In EGC Vent
6
EGC II KOH, LiOH, MSA, or NaOH
1
Deionized Water
NOTE: The EGC Degas fittings cannot be serviced by the user.
Inlet
Outlet
Regen In
8
Regen Out
Eluent
7
EGC Degas
Eluent Out
16 CR-TC
17
From the pulse damper
Degas In
To the inject valve port P(2)
Column Heater Degas Out
13
Suppressor
Cell Out
15
Eluent Out
Regen In
14
Heat Exchanger
Conductivity Cell Cell In
5
Pulse Damper Valve 10
W L
Press. 4 Xducer. C
P
9
3 12
To waste
Eluent Valve
Pump Head
Guard
Pump Head
2
Sample in
Separator
Backpressure Coil
11
L
S
To waste
18
To Gas Separator Assembly
Figure 5-7. ICS-2000 Flow Schematic: KOH, LiOH, MSA, or NaOH Eluent Generation NOTE The numbers on the flow schematic indicate the order in which liquid flows through the system components.
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ICS-2000 Ion Chromatography System
To the pump Degas In EGC Vent 6
NOTE: The EGC degas fittings cannot be serviced by the user
EGC II K2CO3
1
Deionized Water
Inlet
Outlet Eluent Out
8
7
Regen Out
EGC Degas
Eluent In
18
EPM
Regen In
17
Degas In
14
Suppressor
Cell Out
16
Eluent Out
Regen In
15
Heat Exchanger
Regen Out
Eluent In
Degas Out Conductivity Cell Cell In
Column Heater
9
Pulse Damper Valve
L
Press. 4 Xducer.
C P
10
Separator
11
W
12
L
S
13
3
EGC CO3 Mixer
5
19
To waste Pump Head
Guard
Pump Head
To Gas Separator Assembly
2
Sample in
To waste
Eluent Valve
Backpressure Coil
Figure 5-8. ICS-2000 Flow Schematic: Carbonate/Bicarbonate Eluent Generation
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To the pump Degas In EGC Vent 6
NOTE: The EGC degas fittings cannot be serviced by the user
EGC II K2CO3
1
Deionized Water
Inlet
Outlet
7 EGC Degas 16
Degas In
13
Suppressor
Cell Out
15
Eluent Out
Regen In
14
Heat Exchanger
Conductivity Cell Cell In
Regen Out
Eluent In
Degas Out
Column Heater
8
11
L
10
W L
Separator
Pulse Damper Valve
S
Press. 4 Xducer.
C P
12
3
9 Pump Head
2
Sample in To waste
Eluent Valve
Backpressure Coil
To waste Guard
Pump Head
EGC CO3 Mixer
5
17
To Gas Separator Assembly
Figure 5-9. ICS-2000 Flow Schematic: Carbonate Eluent Generation
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5.3
Replacing Tubing and Fittings The ICS-2000 is plumbed with the tubing and tubing assemblies listed below. Tubing Size and Type
Color
Used For
0.125-mm (0.005-in) ID PEEK (P/N 044221)
Red
Connection from pump pulse damper to pressure transducer
0.25-mm (0.010-in) ID PEEK (P/N 042690)
Black
Connections between other system components
0.50-mm (0.020-in) ID PEEK (P/N 042855)
Orange
Connection from injection port to injection valve
0.75-mm (0.030-in) ID PEEK (P/N 044777)
Green
Connection from injection valve to waste
1.58-mm (0.062-in) ID Teflon (P/N 014157)
Clear
Connection from pump to degas or eluent reservoir; pump waste
25 µL sample loop (P/N 042857)
Orange
Connection between ports L (1) and L (4) on the injection valve
•
•
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10-32 fittings (P/N 043275) and ferrules (P/N 043276) are used for most tubing connections. For tightening requirements, refer to Installation of Dionex Liquid Line Fittings (Document No. 031432). The manual is on the Dionex Reference Library CD-ROM (P/N 053891). 1/8-in fittings (P/N 052267) and ferrules (P/N 048949) are used for connections to the suppressor REGEN OUT port and the eluent reservoir.
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5.4
Rebuilding the Injection Valve Dionex recommends rebuilding the injection valve annually. The Injection Valve Rebuild Kit (P/N 057896) contains all required replacement parts. NOTE Substitution of non-Dionex parts may impair valve performance and void the product warranty.
1. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the touch screen HOME page. 2. Open the ICS-2000 front door. 3. Disconnect each liquid line connected to the injection valve. 4. Follow the instructions provided in the Rebuild Kit to replace the rotor seal, isolation seal, and stator face. 5. Reconnect all liquid lines to the injection valve (see Figure 5-10). 6. Close the door. 7. Turn on the pump.
Figure 5-10. Injection Valve Plumbing NOTE A backpressure coil may be installed between Port P and the line labeled TO INJECT VALVE - P.
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5.5
Cleaning and Replacing the Pump Check Valves A dirty check valve causes erratic flow rates and pressures. In addition, it may cause the pump to lose prime and/or be difficult to reprime. If possible, replace dirty check valves. If new check valves are not available, follow the instructions for cleaning. Replacing Check Valves
1. Close the eluent valve from the ICS-2000 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page. 2. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-2000. 3. To prevent contamination of pump parts, put on a pair of rubber gloves before disassembling the pump head. 4. Disconnect the tube fittings from the inlet and outlet check valve assemblies on the primary pump head (see Figure 5-11). 5. Use a 1/2-inch wrench to loosen both check valve assemblies. Remove the check valve assemblies from the pump head.
Outlet Check Valve
Primary Pump Head
Secondary Pump Head
Acorn Nuts
Inlet Check Valve
Figure 5-11. Pump Heads NOTE The inlet check valve assembly housing has a 1/4-28 port. The outlet check valve assembly housing has a 10-32 port.
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6. If you are installing new cartridges (P/N 045994) in the existing check valve housings, place the cartridge in the inlet check valve housing with the double-hole end of the cartridge visible and place the cartridge in the outlet housing with the single-hole end visible. NOTE The pump will not operate properly unless the cartridge is installed in the housing in the correct orientation. Liquid flows through the check valve in the large single hole and out the small double holes.
Double-hole
Inlet Check Valve
Single-hole
Outlet Check Valve
7. Install the inlet check valve assembly (P/N 045722) on the bottom of the primary pump head. Install the outlet check valve assembly (P/N 045721) on the top of the head. Tighten the check valves fingertight, and then use a wrench to tighten an additional one-quarter to one-half turn. Overtightening may damage the pump head and check valve housing and crush the check valve seats.
8. Reconnect the liquid lines. Turn on the ICS-2000 main power. 9. Open the eluent valve from the ICS-2000 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page. 10. Prime the pump (see Section B.13). 11. When the ICS-2000 is at operating pressure, check for leaks from the check valves. Tighten a check valve a little more only if it leaks. Cleaning Check Valves
1. Carefully remove the check valve cartridges from the valve housings. 2. Place the check valve housings and cartridges in a beaker with methanol. Sonicate or agitate the parts for several minutes. 3. Rinse each check valve housing and cartridge thoroughly with filtered deionized water. 4. See Step 6 through Step 11 above to reinstall the check valves and complete the procedure.
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5.6
Replacing a Pump Piston Seal and Piston Rinse Seal A damaged seal allows leakage past the piston, as well as leakage from the piston seal wash housing. The pump may be difficult to prime, flow rates may be unstable, and there may be baseline noise. Preparation
1. Rinse the pump flow path with deionized water. Direct the flow to waste by opening the waste valve on the secondary pump head (see Figure 5-14). To open the valve, turn the knob one-quarter to one-half turn counterclockwise. 2. After rinsing, close the waste valve. 3. Close the eluent valve from the ICS-2000 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page. 4. To prevent contamination of pump parts, put on a pair of rubber gloves before disassembling the pump head. Removing the Head and Piston
1. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-2000. 2. Disconnect all tubing connections to the pump head. 3. Locate the open-end wrench (P/N 014605) provided in the ICS-2000 Ship Kit (P/N 057905). Use the wrench to remove the two acorn nuts (see Figure 5-11) from the pump head. 4. Slowly pull the head and allow it to separate from the housing. Carefully disengage the head from the piston by pulling the head straight off and away from its mounting studs. Lateral motion while disengaging the pump head from the piston may break the piston.
Un mouvement latéral pendant la séparation de la tête et du piston peut casser le piston.
Vermeiden Sie Seitwärtsbewegungen, wenn Sie den Kopf vom Kolben lösen. Andernfalls kann der Kolben brechen.
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5. Place the head (front end down) on a clean work surface and lift off the spacer to expose the piston seal (see Figure 5-12 or Figure 5-13). Priming Valve Knob (P/N 055709) Outlet Check Valve Assembly (P/N 045721) O-Ring (P/N 055752) Piston Seal (P/N 055870) Spacer with Drain (P/N 057913)
Primary Pump Head (P/N 055711)
Piston Rinse Seal (P/N 048722)
O-Ring (P/N 014895) O-Ring (P/N 059283)
Piston (P/N 052840)
Inlet Check Valve Assembly (P/N 045722)
Seal Guide (P/N 058032)
Figure 5-12. Primary Pump Head
Waste Valve Knob (P/N 055710)
O-Ring (P/N 055752) Piston Seal (P/N 055870) Secondary Pump Head (P/N 055712)
Spacer with Drain (P/N 057913) Piston Rinse Seal (P/N 048722) Seal Guide (P/N 058032)
O-Ring (P/N 014895) O-Ring (P/N 059283)
Piston (P/N 052840)
Figure 5-13. Secondary Pump Head
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6. The piston does not come off as part of the pump head assembly because it is captured by a magnetic retention system. After removing the pump head, hold the shaft of the piston (near the base), tilt the piston slightly, and pull the piston away from the pump. Installing the New Piston Rinse Seal
1. Remove the guide from the spacer to expose the piston rinse seal and O-ring. Remove the O-ring. 2. Remove the old piston rinse seal from the guide as follows: a. Hold the guide with the flat side facing up. b. To dislodge the piston rinse seal, gently insert the shaft of the piston through the small hole in the center of the guide (see photo). c. Pull the seal off the end of the piston shaft and remove the piston from the guide. 3. Hold the new piston rinse seal (P/N 048722) with the grooved side facing up. 4. Using your fingertip, gently press the piston rinse seal into the guide until the edge of the seal is below the surface of the guide. The piston rinse seal is made of soft plastic. Do not press on the seal with anything hard or sharp, including your fingernail. If the seal is nicked or gouged, it will not seal properly and may result in leaks.
5. Place the new O-ring (P/N 059283) into the groove in the guide. 6. Remove the O-ring from the groove in the flat side of the spacer and replace it with the new O-ring (P/N 014895). 7. In one hand, hold the guide with the O-ring and piston rinse seal facing up (this prevents the O-ring from falling out). In the other hand, hold the spacer with the cavity facing down. 8. Gently press the guide into the cavity in the spacer until it is fully seated.
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Removing the Piston Seal from the Head
1. Fill the head cavity with deionized water by injecting the liquid through either the piston opening or the inlet check valve. 2. Reinsert the piston approximately 3 mm (0.125) inch into the seal. 3. If this is the primary pump head, install a 10-32 fitting plug (P/N 042772) on the outlet check valve. Tighten the plug. 4. If this is the secondary pump head, install a 10-32 fitting plug (P/N 042772) in both the inlet and outlet ports. Tighten the plugs. 5. Push the piston into the head. (This should hydraulically unseat the seal from the head.) Remove the piston and pull off the seal. NOTE If the piston seal is not removed, make sure the 10-32 fitting plug(s) are tight and add more water. Make sure the head contains no air bubbles, and then repeat Steps 2 and 5.
6. Remove the 10-32 fitting plug(s). Installing the New Piston Seal
1. Open the priming valve knob (primary pump head) or waste valve knob (secondary pump head) by turning the knob one-quarter to one-half turn counterclockwise. 2. Push the piston through the spacer and then through the new seal. Insert the piston and seal into the pump head until the seal makes contact with the bottom of the counterbore. NOTE If necessary, lubricate the seal with a small amount of isopropyl alcohol to facilitate insertion.
3. To seat the seal, push down on the spacer until it is flush with the head. A clicking sound indicates that the seal is correctly seated. 4. Close the priming valve knob or waste valve knob.
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Reinstalling the Head and Piston
Dionex recommends reinstalling the head and piston as a single assembly, so that the piston centers itself onto the magnetic follower. 1. Hold the assembled spacer and guide with the drain tubes aligned vertically and press the spacer into the head until it is flush with the indented surface of the head. 2. Insert the piston so that 1/4 inch of the shaft is exposed. This ensures that the magnet in the follower picks up the piston. (The follower is the cylinder that holds the piston in place as it moves in and out of the pump head assembly.) 3. Reinstall the head and piston assembly; use a wrench to tighten the nuts evenly (12 in-lb torque). Completing the Procedure
1. Reconnect all liquid lines to the pump head. 2. Turn on the main power switch. 3. Open the eluent valve. 4. Prime the pump (see Section B.13).
5.7
Replacing a Pump Piston Continued leaking of the piston seal after installation of a new seal (assuming the pump head is tight) indicates a dirty, scratched, or broken piston. Follow the instructions in Section 5.6 to install a new piston (P/N 052840) and piston seal (P/N 055870).
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5.8
Replacing the Waste Valve or Priming Valve O-Ring A damaged O-ring causes leakage around the base of the waste valve or priming valve knob. 1. Close the eluent valve from the Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page. 2. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-2000. 3. To remove the waste valve or priming valve from the pump head (see Figure 5-14), turn the knob counterclockwise until it is loose, and then pull the knob straight out of the cavity in the pump head.
Priming Valve
Waste Valve
Figure 5-14. Waste and Priming Valves
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4. If the O-ring is removed with the valve knob in Step 3, pull the O-ring off the end of the knob (see Figure 5-15). If the O-ring is not removed with the valve knob, insert a thin object (for example, the bent end of a paper clip) into the cavity in the pump head and carefully pull out the O-ring. Do not scratch the cavity. Scratches in the cavity will cause leaks around the base of the knob while the pump is being primed.
Valve Knob O-Ring (P/N 055752)
Figure 5-15. Waste Valve or Priming Valve O-Ring Replacement
5. Slide a new O-ring (P/N 055752) over the end of the valve. 6. To reinstall the valve containing the new O-ring, turn the knob clockwise and then tighten fingertight. NOTE It is normal to encounter resistance after several rotations of the knob; the O-ring is being pushed into the cavity of the pump head.
7. Turn on the main power switch. 8. Open the eluent valve. 9. Prime the pump (see Section B.13).
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5.9
Replacing the Conductivity Cell 1. Turn off the ICS-2000 power. 2. Open the front door and disconnect the tubing from the CELL IN and CELL OUT fittings (see Figure 5-16, View A). Loosen the two screws on the cell front cover. The screws remain attached (see Figure 5-16, View B).
Unscrew
Disconnect
Unscrew
View B
View A Figure 5-16. Removing the Cell Front Cover
3. Grip the two loosened screws and pull the cell cover toward you to remove it from the component panel. Do not pull from the CELL IN and CELL OUT fittings. 4. Continue pulling on the cover until the attached cell assembly slides out the front of the ICS2000 (see Figure 5-17).
Figure 5-17. Removing the Cell Assembly
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5. Slide the new cell assembly into the opening in the component panel until it stops and the cell cover is flush against the component panel. The cell’s electronic connector automatically plugs into a connector inside the ICS-2000 when you push the assembly into the opening. 6. Tighten the screws on the cell front cover fingertight. 7. Reconnect the inlet and outlet lines. 8. Turn on the ICS-2000 power. 9. Calibrate the new cell in Chromeleon or on the ICS-2000 touch screen DIAGNOSTIC page.Cell calibration of a new cell consists of three parts:
• •
•
Running the offset calibration, which measures the output of the cell electronics alone and determines an offset value to be applied to raw conductivity readings. Running the slope calibration, which measures the output of the cell electronics when a built-in dummy cell, which provides a constant conductivity reading of 21 µS, is automatically enabled. The slope value is applied to raw conductivity readings. Entering the cell constant measured at the factory. The ICS-2000 uses the cell constant to determine the measured conductivity.
To calibrate the cell in Chromeleon: a. Open the Wellness Panel (see Section 5.1.1) b. Under Electric Conductivity Cell Calibration, click Offset Cal. c. When the offset calibration is complete, click Slope Cal. d. Click Calibration Details. Under Conductivity Cell Cal Details, enter the Cell Constant value printed on the front of the cell. e. In the field next to the Download button, verify that Current is selected and then click Download to download the new value to the ICS-2000. f.
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To ensure that the new values are recorded in the ICS-2000 memory, do not turn off the ICS-2000 power for at least 1 minute after downloading.
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To calibrate the cell on the ICS-2000 touch screen DIAGNOSTIC page: a. Go to the DIAGNOSTIC page and touch Electric Conductivity Cell. b. On the ELECTRIC CONDUCTIVITY CALIBRATION page (see Figure 5-18), touch Run Offset Cal.
Figure 5-18. Electric Conductivity Calibration Page
c. When the offset calibration is complete, touch Run Slope Cal. d. Touch the Cell Constant field and enter the value printed on the front of the cell. e. To ensure that the new calibration values are recorded in the ICS-2000 memory, do not turn off the ICS-2000 power for at least 1 minute. f.
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Record the new calibration values in the Chromeleon Wellness database. To do this, open the Wellness Panel (see Section 5.1.1) and click Upload under Update Wellness Database.
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5.10 Replacing the Suppressor Refer to the suppressor manual for guidance about when to replace a suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). 1. Refer to the suppressor quick start guide (shipped with the suppressor) for instructions on preparing the suppressor before initial use and for additional installation details. 2. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the touch screen HOME page. 3. Open the front door of the ICS-2000. 4. Disconnect the two eluent and the two regenerant lines from the suppressor. 5. To remove the suppressor from the component mounting panel, slide it up to detach it from the mounting tabs on the panel and then pull it toward you. 6. Continue pulling the suppressor out until the yellow connector on the cable inside the ICS-2000 is outside the panel (see Figure 5-19). 7. Disconnect the suppressor cable (twist the ring on the yellow connector and pull the two connectors apart).
Yellow Connector
Figure 5-19. Removing the Suppressor
8. Connect the cable from the new suppressor to the ICS-2000 cable (align the pins on the two connectors and push them together). 9. Orient the suppressor with the REGEN OUT fitting on top and the cables to the right.
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10. Push the cables into the opening in the component panel. 11. Align the top of the suppressor with the guide line printed on the component panel (see Figure 5-20) and align the slots on the rear of the suppressor with the tabs on the panel. 12. Press the suppressor onto the tabs and then slide it down until it locks into place. Pull slightly on the center of the suppressor to verify that it is securely fastened. Note: Some suppressors require more force to secure them onto the tabs. 13. Connect the two eluent and two regenerant lines to the new suppressor.
1 Suppressor Mounting Tabs
4
2 Suppressor Cable Connector
3
3 Guideline for AES 4 Guideline for SRS
1
1
2
1
14. Close the ICS-2000 front door. Figure 5-20. Suppressor Guidelines and Mounting Tabs on Component Panel
5.11 Replacing the Column Heater 1. Turn off the ICS-2000 power. 2. Open the front door of the ICS-2000. 3. Follow the steps below to remove the existing column heater: a. Unscrew the two thumbscrews on the heater cover (they remain attached to the cover). b. Pull the heater cover straight out to remove it.
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c. Unscrew the six thumbscrews on the top metal plate (see Figure 5-21) and remove the plate.
Thumbscrews (6)
Figure 5-21. ICS-2000 Column Heater Cover Removed
d. Remove the columns from the column heater. e. Pull the column heater straight toward you to remove it from the component panel. 4. Before installing the new column heater, write down the two calibration values (offset and slope) recorded on the back of the heater. 5. Align the connector on the back of the new column heater (P/N 058060) with the connector on the component panel and push the column heater onto the component panel. 6. Remove the heater cover and the metal plate on the new heater. 7. Install the columns in the new heater and replace the top metal plate and heater cover. 8. Turn on the ICS-2000 power.
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9. Enter the column heater calibration values in Chromeleon or on the ICS-2000 touch screen DIAGNOSTIC page as follows. To enter the calibration values in Chromeleon: a. Open the Wellness Panel (see Section 5.1.1) and click Calibration Details. b. Under Column Heater Calibration Values, enter the Column Heater Offset and Column Heater Slope values recorded in Step 4. c. In the field next to the Download button, verify that Current is selected and then click Download to download the new calibration values to the ICS-2000. d. To ensure the new calibration values are recorded in the ICS-2000 memory, do not turn off the ICS-2000 power for at least 1 minute after downloading the values. To enter the calibration values on the ICS-2000 touch screen DIAGNOSTIC page: a. Go to the DIAGNOSTIC page and touch Column Heater Cal Values. b. On the COLUMN HEATER CAL VALUES page (see Figure 5-22), enter the Calibrated Offset and Calibrated Slope values recorded in Step 4.
Figure 5-22. Column Heater Cal Values Page
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c. To ensure the calibration values are recorded in the ICS-2000 memory, do not turn off the ICS-2000 power for at least 1 minute after entering the values. d. Record the calibration values in the Chromeleon Wellness database. To do this, open the Wellness Panel (see Section 5.1.1) and click Upload under Update Wellness Database.
5.12 Replacing the Column Heater Heat Exchanger 1. Turn off the ICS-2000 power. 2. Open the front door of the ICS-2000. 3. Unscrew the two thumbscrews on the column heater cover (they remain attached to the cover).
Thumbscrews (6) Heat Exchanger Screws (3)
4. Pull the heater cover straight out to remove it. 5. Unscrew the six thumbscrews on the top metal plate (see Figure 5-23) and remove the plate. 6. Disconnect the heat exchanger inlet line from Port C on the injection valve. Figure 5-23. ICS-2000 Column Heater Cover Removed
7. Disconnect the heat exchanger outlet line from the guard column inlet. 8. Use an Allen wrench to remove the three screws from the heat exchanger metal plate and remove the plate (with the tubing) from the heater. 9. Remove the plastic backing from the new heat exchanger (P/N 059979, with 0.25-mm (0.010-in) ID tubing; P/N 060943, with 0.125-mm (0.005-in) ID
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tubing) and press the heat exchanger onto the heater. Replace the screws removed in Step 8. 10. Connect the new heat exchanger inlet line to Port C on the injection valve and connect the outlet line to the guard column inlet. 11. Reinstall the top metal plate and the heater cover.
5.13 Replacing the Eluent Valve 1. Turn off the power to the ICS-2000. 2. Open the ICS-2000 front door. 3. To prevent an eluent leak during the valve replacement procedure, disconnect the eluent line from the reservoir cap. Or, plug the line on the left side of the valve with a coupler (P/N 039056 and a plug (P/N 037268) after disconnecting the liquid line from the valve (see Step 4). 4. Disconnect the two liquid lines connected to the eluent valve (see Figure 5-24).
Disconnect
5. Unscrew and remove the two screws that attach the valve to the component panel (see Figure 5-24). Save the screws.
Remove
Figure 5-24. Eluent Valve
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6. Pull the valve straight out from the component panel and begin pulling the attached cable out of the opening in the panel. 7. The cable is connected to a matching cable inside the ICS2000. Continue pulling until the connectors for the two cables are outside the panel (see Figure 5-25). Disconnect the cables.
Eluent Valve Cable Disconnect Cables
Figure 5-25. Eluent Valve Cable
8. Remove the mounting plate on the old valve by unscrewing and removing the two screws. Save the screws. 9. Thread the cable from the new eluent valve through the mounting plate.
Remove Screws
10. Attach the mounting plate to the new valve using the screws removed in Step 8. Figure 5-26. Removing the Valve Mounting Plate
11. Connect the cable from the new valve (P/N 057945) to the ICS-2000 cable. Feed the cables back inside the ICS-2000. 12. Align the new valve on the component panel with the liquid ports facing up and attach it with the two screws removed in Step 5. Reconnect the liquid lines. 13. Turn on the power to the ICS-2000. 14. Prime the pump (see Section B.13).
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5.14 Replacing the Leak Sensor 1. Turn off the power to the ICS2000. 2. Open the ICS-2000 front door. 3. Loosen the screw on the front of the leak sensor (see Figure 5-27). Note: The screw remains attached to the sensor. Leak Sensor
Loosen Screw
Figure 5-27. Leak Sensor
4. Remove the leak sensor from the component panel and pull the cable out of the opening in the panel. 5. The cable attached to the leak sensor is connected to a matching cable inside the ICS2000. Continue pulling the cable until the connectors for the two cables are outside of the panel (see Figure 5-28).
Disconnect Cables
6. Disconnect the two cables. Figure 5-28. Leak Sensor Cable
7. Connect the cable from the new leak sensor (P/N 058053) to the ICS-2000 cable. 8. Feed the cables back inside the ICS-2000. Align the leak sensor with the component panel opening and fingertighten the screw. 9. Make sure the leak sensor does not touch the bottom of the drip tray.
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5.15 Priming the Pump with Isopropyl Alcohol NOTE Prime the pump heads with isopropyl alcohol only if the two standard priming procedures described in Section B.13 are unsuccessful.
1. Connect a 10-mL syringe (P/N 054578) filled with isopropyl alcohol (IPA) to the port in the primary pump head (see Figure 5-29). 2. Open the waste valve on the secondary pump head (see Figure 5-29) by turning the knob onequarter to one-half turn counterclockwise.
Secondary Pump Head
Waste Valve (open) Port Primary Pump Head
10 mL Syringe (P/N 054578)
Priming Valve (open)
Figure 5-29. Priming the Pump Heads with IPA
3. Click Pump On on the Chromeleon Control panel to turn on the pump motor. 4. Open the priming valve on the primary pump head by turning it one-quarter to one-half turn counterclockwise. 5. Use the syringe to slowly push alcohol through the pump. NOTE Be careful not to push any air trapped in the syringe through the pump. Check the waste line from the secondary pump head to verify that there are no air bubbles.
6. Close the priming valve. Do not overtighten. Disconnect the syringe from the priming valve. 7. Let the pump run for several minutes, to purge alcohol from the pump heads, and then click Prime and flush the heads with the desired eluent.
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Isopropyl alcohol may damage some columns. Be sure to thoroughly rinse the alcohol from the pump, using the process described in Step 7.
8. Close the waste valve. Do not overtighten. 9. Select the flow rate required for the analysis. 10. Click Pump Off to turn off the pump motor. The pump is now ready for operation.
5.16 Changing Main Power Fuses 1. Turn off the main power switch. HIGH VOLTAGE—Disconnect the main power cord from its source and also from the rear panel of the ICS-2000. HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa source et du panneau arrière du ICS-2000.
HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der Rückseite des ICS-2000.
2. The fuse holder is part of the main power receptacle (see Figure 5-30) on the ICS-2000 rear panel. To remove the fuse holder, squeeze the tab on the top of the holder to release it and pull the holder straight out of its compartment.
Figure 5-30. Main Power Fuse Holder
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3. Replace the two fuses in the holder with new IEC 127 fast-blow fuses rated 3.15 amps (P/N 954745). Dionex recommends always replacing both fuses. 4. Reinsert the fuse holder into its compartment and push in until the tab clicks in place. 5. Reconnect the main power cord and turn on the power.
5.17 Replacing an EluGen Cartridge The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), or a corrosive acid (MSA). Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), ou un acide corrosif (MSA). Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), oder eine korrodierende Säure (MSA). Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
The procedure for replacing an EluGen cartridge differs, depending on the type of cartridge:
• •
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To replace a KOH, LiOH, MSA, or NaOH EluGen cartridge, go to Section 5.17.1. To replace a K2CO3 cartridge, go to Section 5.17.2
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5.17.1 Replacing a KOH, LiOH, MSA, or NaOH EluGen Cartridge 1. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the ICS-2000 touch screen HOME page. 2. Disconnect the EluGen cartridge cable from the EGC-1 connector on the ICS-2000 top cover. 3. Disconnect the CR-TC cable from the CR-TC connector. 4. Remove the EluGen cartridge VENT line (see Figure 5-31) from the EluGen cartridge by unscrewing the luer lock from the luer adapter.
Luer Adapter Luer Lock
EGC Vent Line
If necessary, use a wrench to hold the luer adapter in place while unscrewing the vent line. Figure 5-31. EluGen Cartridge Vent Line and Luer Fitting
5. Install the luer cap (P/N 053981), provided with the EluGen cartridge, onto the luer adapter. This prevents leaks from the vent opening when you turn over the EluGen cartridge (see Step 7). 6. Lift the EluGen cartridge straight up and out of the cartridge holder.
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7. Turn the cartridge upside down and set it in the EluGen cartridge service area on top of the ICS-2000 (see Figure 5-32 and Figure 5-33).
EluGen Cartridge Service Area
Figure 5-32. EluGen Cartridge Service Area
Figure 5-33. EluGen Cartridge in the Service Area
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8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the EluGen cartridge (see Figure 5-34).
EGC OUT OUTLET Port
EGC IN INLET Port
Figure 5-34. Disconnect the EluGen Cartridge Inlet and Outlet Port Lines
9. Follow the instructions in the EluGen cartridge manual, provided on the Dionex Reference Library CD-ROM (P/N 053891), to prepare an expended EluGen cartridge for disposal or to store a partially used EluGen cartridge for later use. 10. Remove the new EluGen cartridge from the shipping box. 11. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the EluGen cartridge INLET and OUTLET ports (see Figure 5-35).
OUTLET
INLET
Figure 5-35. EluGen Cartridge Inlet and Outlet Ports
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12. Set the EluGen cartridge in the service area on top of the ICS-2000 and orient it with the cable toward the EGC holder (see Figure 5-36).
EluGen Cartridge Cable
Figure 5-36. EluGen Cartridge in Service Area
13. Connect EGC IN to the EluGen cartridge INLET port. 14. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) in the ICS-2000 Ship Kit (P/N 064375). 15. Connect one end of this coil to the EluGen cartridge OUTLET port (see Figure 5-37). Leave the other end of the coil unconnected.
Backpressure Coil OUTLET Port
Figure 5-37. EluGen Cartridge Outlet Connection for Conditioning the Cartridge
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NOTE The backpressure coil connection is temporary; it is used only during the EluGen cartridge conditioning procedure described in “Conditioning the EluGen Cartridge” on page 5-46.
16. Turn the EluGen cartridge over, with the fittings facing down. Shake the EluGen cartridge vigorously and tap it with the palm of your hand 10 to 15 times. Check that all bubbles trapped in the eluent generation chamber are dislodged. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), or a corrosive acid (MSA). Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), ou un acide corrosif (MSA). Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), oder eine korrodierende Säure (MSA). Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
17. Slide the EluGen cartridge down into the holder until it stops. Make sure the cable and backpressure coil remain out of the holder (see Figure 5-38). NOTE To avoid crimping the lines inside the holder, do not twist the cartridge before you slide it into the holder. The lines are designed to coil inside the holder.
Figure 5-38. Installing the EluGen Cartridge in the Holder
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18. Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure 5-39. Push it onto the EGC-1 connector on the ICS2000. Twist the ring on the cable connector fingertight to secure it.
Figure 5-39. Connecting the EluGen Cartridge Cable
19. Remove the plug from the EluGen cartridge vent opening and connect the EluGen cartridge VENT line.
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Recording the EluGen Cartridge Serial Number in Chromeleon
The serial number is printed on the EluGen cartridge label. 1. Open the Chromeleon Server Configuration program (select Start > Programs (or All Programs) > Chromeleon > Server Configuration). 2. Double-click the ICS-2000 system icon. The properties dialog box for the ICS-2000 appears. 3. Click the Eluent Generator tab (see Figure 5-40). 4. Select the EGC-1 check box. 5. Enter the EluGen cartridge serial number and click OK.
Figure 5-40. Eluent Generator Configuration Properties Example
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Conditioning the EluGen Cartridge
Always condition the EluGen cartridge before initial use. This requires directing the backpressure coil connected to the EluGen cartridge outlet to waste, and then generating 50 mM of eluent at 1.00 mL/min for 30 minutes. Follow the steps below: 1. Set a temporary waste container, such as a beaker, on top of the ICS2000 and direct the yellow backpressure coil from the EluGen cartridge OUTLET port to the container. 2. From the Chromeleon Control panel or the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min and set the EluGen cartridge concentration to 50 mM. 3. Verify that the suppressor and CR-TC are off. To avoid damaging the suppressor and CR-TC, always turn off the suppressor and CR-TC before conditioning the EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor or CR-TC.
4. Verify that the Automatically turn on with pump options are not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9) and ELUENT GENERATOR page (see Section C.8). Disabling these options lets you turn on the pump, without automatically turning on the suppressor and CR-TC. 5. Verify that the eluent reservoir is filled with ASTM filtered, Type 1 (18 megohm-cm) deionized water. 6. Turn on the pump. 7. Run at the selected settings (1.00 mL/min at 50 mM) for 30 minutes. 8. Turn off the pump. 9. Disconnect the EluGen cartridge cable. 10. Remove the backpressure tubing from the waste container and remove the waste container.
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11. Lift the EluGen cartridge out of the holder, turn it over, and set it in the service area.
EGC OUT EGC IN
OUTLET Port
INLET Port
12. Disconnect the backpressure coil from the EluGen cartridge OUTLET port. 13. Connect the EGC OUT line from the holder to the OUTLET port (see Figure 5-41). Figure 5-41. EluGen Cartridge Inlet and Outlet Connections
14. Turn over the EluGen cartridge (fittings facing down). Check for bubbles. If necessary, shake and tap the EluGen cartridge to remove bubbles. 15. Reinstall the EluGen cartridge in the holder. 16. Reconnect the EluGen cartridge cable. 17. Reconnect the CR-TC cable. 18. If you disabled the Automatically turn on with pump option in Step 3, select the option.
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5.17.2 Replacing a K2CO3 Cartridge 1. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the ICS-2000 touch screen HOME page. 2. Disconnect the EluGen cartridge cable from the EGC-1 connector on the ICS-2000 top cover. 3. If an EPM is installed, disconnect the EPM cable from the EGC-2 connector. 4. Remove the EluGen cartridge VENT line (see Figure 5-31) from the EluGen cartridge by unscrewing the luer lock from the luer adapter.
Luer Adapter Luer Lock
EGC Vent Line
If necessary, use a wrench to hold the luer adapter in place while unscrewing the vent line. Figure 5-42. EluGen Cartridge Vent Line and Luer Fitting
5. Install the luer cap (P/N 053981), provided with the EluGen cartridge, onto the luer adapter. This prevents leaks from the vent opening when you turn over the EluGen cartridge (see Step 7). 6. Lift the EluGen cartridge straight up and out of the cartridge holder.
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7. Turn the cartridge upside down and set it in the EluGen cartridge service area on top of the ICS-2000 (see Figure 5-32 and Figure 5-33).
EluGen Cartridge Service Area
Figure 5-43. EluGen Cartridge Service Area
Figure 5-44. EluGen Cartridge In the Service Area
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8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET fittings on the EluGen cartridge (see Figure 5-34).
EGC OUT OUTLET Port
EGC IN INLET Port
Figure 5-45. Disconnect the EluGen Cartridge Inlet and Outlet Port Lines
9. Follow the instructions in the EluGen cartridge manual, provided on the Dionex Reference Library CD-ROM (P/N 053891), to prepare an expended EluGen cartridge for disposal or to store a partially used EluGen cartridge for later use. 10. Remove the new EluGen cartridge from the shipping box. 11. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the EluGen cartridge INLET and OUTLET ports (see Figure 5-35).
OUTLET
INLET
Figure 5-46. EluGen Cartridge Inlet and Outlet Ports
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12. Set the EluGen cartridge in the service area on top of the ICS-2000 and orient it with the cable toward the EGC holder (see Figure 5-36).
EluGen Cartridge Cable
Figure 5-47. EluGen Cartridge in Service Area
13. Connect EGC IN to the EluGen cartridge INLET port. 14. Connect EGC OUT to the EluGen cartridge OUTLET port. 15. Turn the EluGen cartridge over (with the fittings facing down). Shake the EluGen cartridge vigorously, and tap it with the palm of your hand 10 to 15 times. Check that all bubbles trapped in the eluent generation chamber are dislodged. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution concentrée de K2CO3. Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), eine korrodierende Säure (MSA) oder eine konzentrierte K2CO3-Lösung. Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
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16. Slide the EluGen cartridge down into the holder until it stops (see Figure 5-48). Make sure the cable remains out of the holder. NOTE To avoid crimping the lines, do not twist the cartridge when you slide it into the holder. The lines are designed to coil inside the holder.
Figure 5-48. EluGen Cartridge Installed in the Holder
17. Remove the plug from the EGC-1 connector on top of the ICS-2000. 18. Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure 5-49. Push it onto the EGC-1 connector on the ICS2000. Twist the ring on the cable connector fingertight to secure it.
Figure 5-49. Connecting the EluGen Cartridge Cable
19. Remove the plug from the EluGen cartridge vent opening and connect the EluGen cartridge VENT line.
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Recording the EluGen Cartridge Serial Number in Chromeleon
The serial number is printed on a label on the EluGen cartridge. 1. Open the Server Configuration program (select Start>Programs (or All Programs)>Chromeleon>Server Configuration). 2. Double-click the ICS-2000 system icon. The properties dialog box for the ICS-2000 appears. 3. Click the Eluent Generator tab. 4. Select the EGC-1 check box. 5. Enter the EluGen cartridge serial number. Verify that the cartridge type is Carb. If not, make sure the cartridge serial number has been entered correctly. Continue on to one of the following sections, depending on the type of eluent to be generated:
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For carbonate eluent, go to “Plumbing the EluGen Cartridge for Conditioning with Carbonate Eluent” on page 5-54. For carbonate/bicarbonate eluent, go to “Plumbing the EluGen Cartridge and EPM for Conditioning with Carbonate/Bicarbonate Eluent” on page 5-57.
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Plumbing the EluGen Cartridge for Conditioning with Carbonate Eluent
Figure 5-50 illustrates the liquid flow path during the EluGen cartridge conditioning procedure with carbonate eluent. EGC VENT
EGC II K2CO3
Send to waste Outlet
Inlet EGC IN
TO DEGAS ELUENT IN TO DEGAS ELUENT OUT
EGC OUT
EGC DEGAS
TO EGC CO3 MIXER OUT
TO INJ VALVE IN - P/ ELUENT OUT
TO PUMP/ DAMPER
14 MPa (2000 psi) at 1.0 mL/min
Backpressure Coil
Pre-plumbed to Pump Pulse Damper To waste
WASTE, GAS SEPARATOR
EGC CO3 Mixer
Temporarily disconnect from TO INJ VALVE IN - P/ ELUENT OUT
TO INJ VALVE PORT P
TO EGC CO3 MIXER IN
TO SRS/AES REGEN OUT
Connected to Connected to Connected to Inject Valve Suppressor Gas Separator Regen Out Assembly Port P (2)
Figure 5-50. EluGen Cartridge Plumbing for Conditioning with Carbonate Eluent
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1. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from the EGC CO3 Mixer inlet. 2. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) and a 10-32 to 10-32 coupler (P/N 042627) in the ICS2000 Ship Kit (P/N 064375). 3. Use the coupler to connect the TO INJ VALVE IN - P/ELUENT OUT line to one end of the backpressure coil (see Figure 5-51). 4. Direct the free end of the backpressure coil to a temporary waste container.
EGC Cable
TO INJ VALVE IN - P/ ELUENT OUT
Backpressure Coil
Temporary Waste Container
Figure 5-51. Plumbing Connections for Conditioning the EluGen Cartridge with Carbonate Eluent
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Conditioning the EluGen Cartridge
Always condition the EluGen cartridge for 30 minutes before initial use. 1. Make sure the eluent reservoir is filled with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before conditioning the EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor.
3. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 4. From the ICS-2000 Control panel in Chromeleon or the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min. 5. Turn on the pump. 6. From the Chromeleon Control panel or the touch screen ELUENT GENERATOR page, set the EGC-1 concentration to 9 mM. 7. Turn on the EGC-1 current. 8. Run at these settings for 30 minutes. 9. Turn off the EGC-1 current. 10. Turn off the pump. 11. Remove the backpressure coil. 12. Reconnect the TO INJ VALVE IN - P/ELUENT OUT line to the mixer inlet.
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Plumbing the EluGen Cartridge and EPM for Conditioning with Carbonate/Bicarbonate Eluent
Figure 5-52 illustrates the liquid flow path through the eluent generator during conditioning with carbonate/bicarbonate eluent.
EGC VENT
EGC II K2CO3
Send to waste
Inlet EGC IN
Outlet EGC OUT
TO CR-TC/EPM ELUENT OUT (yellow label)
(yellow label)
EGC DEGAS
TO DEGAS ELUENT OUT
M /EP -TC UT CR EN O el) TO EG lab R lue (b
ELUENT IN
TO DEGAS ELUENT IN
TO EL CR(re UE TC/ d NT EP lab IN M el )
(red label)
EPM
TO EGC CO3 MIXER OUT TO CR-TC/EPM REGEN IN (orange label) TO PUMP/ DAMPER
EGC CO3 Mixer
(blue label)
WASTE, GAS SEPARATOR
TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
Backpressure Coil 14 MPa (2000 psi) at 1.0 mL/min
TO INJ VALVE PORT P
TO EGC CO3 MIXER IN
Temporarily disconnect from TO INJ VALVE IN P/ELUENT OUT
Connected to Gas Separator Assembly
Connected to Inject Valve Port P (2) TO SRS/AES REGEN OUT
10-32 to 1/4-28 Coupler
Figure 5-52. Plumbing for Conditioning with Carbonate/Bicarbonate Eluent
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1. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) and 10-32 to 1/4-28 coupler (P/N 042806) in the ICS2000 Ship Kit (P/N 064375). 2. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from the EGC CO3 Mixer inlet. 3. Connect one end of the backpressure coil to the TO INJ VALVE IN P/ELUENT OUT line. 4. Connect the 10-32 to 1/4-28 coupler to the free end of the backpressure coil. 5. Disconnect the TO SRS/AES REGEN OUT line from the suppressor REGEN OUT port. 6. Connect the TO SRS/AES REGEN OUT line to the 10-32 to 1/4-28 coupler (see Figure 5-53). NOTE The backpressure coil connection in Figure 5-53 is temporary; it is required only during the conditioning procedure described in the next section.
TO SRS/AES REGEN OUT
10-32 to 1/4-28 coupler
Backpressure Coil
10-32 to 10-32 coupler
TO INJ VALVE IN - P/ ELUENT OUT
Figure 5-53. Backpressure Coil Connections for Conditioning the EPM with Carbonate/Bicarbonate Eluent
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Conditioning the EluGen Cartridge
Always condition the EluGen cartridge for 30 minutes before initial use. 1. Make sure the eluent reservoir is filled with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before conditioning the EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor.
3. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 4. From the ICS-2000 Control panel in Chromeleon or the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min. 5. Turn on the pump. 6. Select the following settings from the Chromeleon Control panel or the touch screen ELUENT GENERATOR page:
•
Set the EGC-1 concentration to 9 mM.
•
Set the EGC-2 concentration to 1 mM.
7. Turn on the EGC-1 and EGC-2 currents. 8. Run at these settings for 30 minutes. 9. Turn off the EGC-1 and EGC-2 currents. 10. Turn off the pump. 11. Remove the backpressure coil. 12. Reconnect the TO INJ VALVE IN - P/ELUENT OUT line to the mixer inlet. 13. Reconnect the TO SRS/AES REGEN OUT line to the suppressor REGEN OUT port.
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5.18 Replacing the CR-TC 1. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the touch screen HOME page. 2. Follow the instructions in Section 5.17.1, Step 2 through Step 8 to disconnect the EluGen cartridge and CR-TC cables, cap the EluGen cartridge vent opening, remove the EluGen cartridge from the holder, and disconnect the inlet and outlet tubing. 3. Disconnect the line labeled TO INJ VALVE IN - P/ELUENT OUT from port P (2) on the injection valve and disconnect the line labeled SRS/AES REGEN OUT from the REGEN OUT port on the suppressor. 4. Lift up the holder and tilt it to view the bottom of the holder.
Disconnect liquid lines from 4 ports
5. Brace the holder against the back corner of the ICS-2000. 6. Grasp the top of the CR-TC and lift up to disconnect it from the holder. 7. Disconnect the liquid lines from the four ports on the CR-TC (see Figure 5-54).
Figure 5-54. Disconnecting CR-TC Liquid Lines
8. Remove the CR-TC from the holder. 9. Remove the plugs from the ports on the new CR-TC (P/N 060477, anion; P/N 060478, cation). Reconnect the liquid lines that were disconnected in Step 7 to the corresponding ports on the new CR-TC.
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10. Check that none of the lines are caught under the CR-TC and then push the CR-TC onto the metal stud inside the EGC holder. Push down until the CR-TC snaps into place (see Figure 5-55).
Figure 5-55. CR-TC Installed in Holder
11. Feed the CR-TC cable through the slot on the side of the EGC holder (see Figure 5-56). 12. Turn the EGC holder right-side up.
CR-TC Cable
Figure 5-56. CR-TC Cable
13. Reconnect the EGC IN and EGC OUT lines to the EluGen cartridge inlet and outlet ports. 14. Turn over the EluGen cartridge (fittings facing down). Check for bubbles in the eluent generation chamber; if necessary, shake and tap the EluGen cartridge to remove bubbles.
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15. Reinstall the EluGen cartridge in the holder. 16. Remove the cap on the luer adapter by twisting. Save the cap. 17. Twist the luer lock and EGC VENT line into the luer adapter. 18. Do not connect the EluGen cartridge cable until after hydrating the CR-TC. Hydrating the CR-TC
The CR-TC must be hydrated before initial use by running ASTM filtered, Type 1 (18 megohm-cm) deionized water through the CR-TC for 10 minutes, while bypassing the columns and suppressor. Figure 5-57 illustrates the liquid flow path through the CR-TC during the hydration procedure. Deionized water in from pump TO EGC OUT
TO DEGAS ELUENT OUT
EGC DEGAS CR-TC
Eluent Out
Regen Out Eluent In
TO DEGAS ELUENT IN
Regen In
TO CR-TC ELUENT IN (red)
TO CR-TC REGEN OUT TO (blue) RE C R (o GE -TC ra N ng IN e)
TO CR-TC/EPM ELUENT OUT (yellow)
DEGAS ELUENT OUT
WASTE, GAS SEPARATOR
10-32 to 1/4-28 Coupler TO INJ VALVE IN - P/ ELUENT OUT
TO SRS/AES REGEN OUT
Figure 5-57. CR-TC Plumbing for Hydration
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1. Locate the 10-32 to 1/4-28 coupler (P/N 042806) in the ICS-2000 Ship Kit (P/N 064375). 2. Use the coupler to connect the line labeled TO INJ VALVE IN P/ELUENT OUT and the line labeled SRS/AES REGEN OUT. 3. Verify that the current to the suppressor is turned off. To avoid damaging the suppressor, always turn off the suppressor before hydrating the CR-TC. The pump flow is on during hydrating, however, no flow reaches the suppressor.
4. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen ELUENT GENERATOR page (see Section C.8). Disabling this option lets you turn on the pump, without automatically turning on the CR-TC. 5. Turn on the pump and set the flow to the rate recommended for your application. Pump deionized water through the CR-TC for at least 10 minutes. 6. Turn off the pump and disconnect the coupler. 7. Reconnect the line labeled TO INJ VALVE IN - P/ELUENT OUT to port (P) 2 on the injection valve. 8. Reconnect the line labeled TO SRS/AES REGEN OUT to the REGEN OUT port on the suppressor. 9. Reconnect the CR-TC and EluGen cartridge cables. 10. If you disabled the Automatically turn on with pump option in Step 3, select the option.
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5.19 Replacing the EPM Electrolytic pH Modifier 1. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the touch screen HOME page. 2. Disconnect the EPM electrical cable from the EGC-2 connector on the ICS2000 top cover. 3. Disconnect the four liquid lines from the ports on the EPM. 4. Lift up the mounting bracket with the EPM attached and remove the bracket and EPM from the EGC holder. 5. Pull the EPM off the mounting bracket. 6. Remove the plugs from the ports on the new EPM (P/N 063175). 7. Push the EPM onto the ball studs on the mounting bracket (see Figure 5-58).
EPM
Mounting Bracket EGC Cable
Ball Studs
Figure 5-58. EPM and Mounting Bracket
8. Reinstall the mounting bracket with new EPM attached onto the EGC holder. 9. Reconnect the liquid lines that were disconnected in Step 3 to the corresponding ports on the new EPM. 10. Connect the EPM electrical cable to the EGC-2 connector.
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5.19.1 Recording the EPM Serial Number in Chromeleon The serial number is printed on a label on the EPM. 1. Open the Server Configuration program (select Start > Programs (or All Programs) > Chromeleon > Server Configuration). 2. Double-click the ICS-2000 system icon. The properties dialog box for the ICS-2000 appears. 3. Click the Eluent Generator tab (see Figure 5-40). 4. Select the EGC-2 check box. 5. Enter the serial number of the EPM. 6. Verify that the cartridge type is pH Mod. If not, make sure the serial number was entered correctly. 7.
Click OK.
Figure 5-59. Eluent Generator Configuration Properties Example
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5.19.2 Plumbing the EPM for Hydrating and Conditioning Figure 5-52 illustrates the liquid flow path during hydration and conditioning.
EGC VENT
EGC II K2CO3
Send to waste
Inlet EGC IN
Outlet EGC OUT
TO CR-TC/EPM ELUENT OUT (yellow label)
(yellow label)
EGC DEGAS
TO DEGAS ELUENT OUT
M /EP -TC UT CR EN O el) TO EG lab R lue (b
ELUENT IN
TO DEGAS ELUENT IN
TO EL CR(re UE TC/ d NT EP lab IN M el )
(red label)
EPM
TO EGC CO3 MIXER OUT TO CR-TC/EPM REGEN IN (orange label) TO PUMP/ DAMPER
EGC CO3 Mixer
(blue label)
WASTE, GAS SEPARATOR
TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
Backpressure Coil 14 MPa (2000 psi) at 1.0 mL/min
TO INJ VALVE PORT P
TO EGC CO3 MIXER IN
Temporarily disconnect from TO INJ VALVE IN P/ELUENT OUT
Connected to Gas Separator Assembly
Connected to Inject Valve Port P (2) TO SRS/AES REGEN OUT
10-32 to 1/4-28 Coupler
Figure 5-60. EluGen Cartridge and EPM Plumbing for Conditioning
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1. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from the EGC CO3 Mixer inlet. 2. Use a 10-32 to 10-32 coupler (P/N 042627) to connect the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) to the TO INJ VALVE IN - P/ELUENT OUT line. 3. Connect a 10-32 to 1/4-28 coupler (P/N 042806) to the free end of the backpressure coil. 4. Disconnect the TO SRS/AES REGEN OUT line from the suppressor REGEN OUT port. 5. Connect the TO SRS/AES REGEN OUT line to the 10-32 to 1/4-28 coupler (see Figure 5-61). NOTE The backpressure coil connection in Figure 5-61 is temporary; it is used only during the hydration and conditioning procedure described in the next section.
TO SRS/AES REGEN OUT
10-32 to 1/4-28 coupler
Backpressure Coil
10-32 to 10-32 coupler
TO INJ VALVE IN - P/ ELUENT OUT
Figure 5-61. Backpressure Coil Connections for Hydrating and Conditioning the EPM with Carbonate Eluent
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5.19.3 Hydrating and Conditioning the EPM Follow the steps below to hydrate the EPM for 5 minutes and then condition the EPM for 30 minutes. 1. Fill the eluent reservoir with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before conditioning the EPM and EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor.
3. Verify that the EluGen cartridge is off. 4. Verify that the Automatically turn on with pump options are not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9) and ELUENT GENERATOR page (see Section C.8). Disabling these options lets you turn on the pump, without automatically turning on the suppressor and EluGen cartridge. 5. From the ICS-2000 Control panel in Chromeleon or the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min. 6. Turn on the pump. 7. Run the pump for 5 minutes to hydrate the EPM. 8. Select the following settings from the Chromeleon Control panel or the touch screen ELUENT GENERATOR page:
•
Set the EGC-1 concentration to 9 mM.
•
Set the EGC-2 concentration to 1 mM.
9. Turn on the EGC-1 and EGC-2 currents. 10. Run at these settings for 30 minutes. 11. Turn off the EGC-1 and EGC-2 currents. 12. Turn off the pump. 13. Remove the backpressure coil and couplers from the TO INJ VALVE IN - P/ELUENT OUT and TO SRS/AES REGEN OUT lines. 14. Reconnect the TO INJ VALVE IN - P/ELUENT OUT line to the EGC CO3 Mixer inlet.
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15. Reconnect the TO SRS/AES REGEN OUT line to the suppressor REGEN OUT port.
5.20 Replacing the EGC CO3 Mixer 5.20.1 Installing the New EGC CO3 Mixer 1. Turn off the pump from the ICS-2000 Control panel in Chromeleon or from the touch screen HOME page. 2. Disconnect the inlet and outlet lines (labeled TO EGC CO3 MIXER IN and TO EGC CO3 MIXER OUT) from the existing mixer and pull the mixer off the mounting clips. 3. Orient the new EGC CO3 Mixer (P/N 061686) with the outlet pointing upward and push it onto the mounting clips (see Figure 5-62). The mixer outlet must point upward to ensure thorough mixing of the eluent.
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4. Connect the TO EGC CO3 MIXER IN line to the mixer inlet and connect the TO EGC CO3 MIXER OUT line to the mixer outlet.
TO EGC CO3 MIXER OUT
TO EGC CO3 MIXER IN
Figure 5-62. ICS-2000 with an EGC CO3 Mixer Installed
5.20.2 Filling the EGC CO3 Mixer with Deionized Water Before initial use, follow the steps below to temporarily fill the EGC CO3 Mixer with deionized water. Then, follow the steps in the next section to fill the mixer with eluent of the required concentration for the application to be run. 1. Verify that the EGC-1 and EGC-2 currents are off. 2. Disconnect the EluGen cartridge inlet line (labeled TO PUMP/DAMPER) from the coupler that connects it to the green pump outlet line (see Figure 5-63).
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TO PUMP/ DAMPER (disconnect this line)
Pump Outlet (green tubing)
Figure 5-63. Disconnect the Cartridge Inlet and Pump Outlet
3. Disconnect the TO EGC CO3 MIXER IN line from the TO INJ VALVE IN P/ELUENT OUT line.
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4. Connect the pump outlet to the mixer inlet (see Figure 5-64).
Pump Outlet
Mixer Inlet
Figure 5-64. Pump Outlet Connected to Mixer Inlet for Mixer Hydration
5. Disconnect the mixer outlet line (labeled TO INJ VALVE PORT P) from port P (2) on the injection valve. 6. Direct the mixer outlet line to a temporary waste container, such as a beaker. 7. From the ICS-2000 Control panel in Chromeleon or the ICS-2000 touch screen HOME page, set the pump flow rate to 5.00 mL/min. 8. Verify that the suppressor is off. To avoid damaging the suppressor always turn off the suppressor before filling the mixer. The pump flow is on during filling, however, no flow reaches the suppressor.
9. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 10. Turn on the pump. 11. Run the pump until the mixer is filled and there is a consistent flow of water exiting the mixer outlet.
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It takes about 5 minutes to fill a 4-mm mixer and about 2 minutes to fill a 2-mm mixer. 12. Turn off the pump.
5.20.3 Filling the EGC CO3 Mixer with Eluent Before initial use, follow the steps in this section to fill the EGC CO3 Mixer with the eluent required for the application to be run. The procedure varies slightly, depending on the type of eluent to be generated:
• •
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For carbonate eluent, see “Filling the EGC CO3 Mixer with Carbonate Eluent” below. For carbonate/bicarbonate eluent, see “Filling the EGC CO3 Mixer with Carbonate/Bicarbonate Eluent” on page 5-77.
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Filling the EGC CO3 Mixer with Carbonate Eluent
Figure 5-65 illustrates the liquid flow path through the eluent generator components during initial filling of the EGC CO3 Mixer with carbonate eluent. EGC IN
To the EluGen cartridge inlet port
TO DEGAS ELUENT IN
EGC OUT
From the EluGen cartridge outlet port
EGC DEGAS
TO DEGAS ELUENT OUT
TO EGC CO3 MIXER OUT
TO INJ VALVE IN - P/ ELUENT OUT
EGC CO 3 Mixer
WASTE, GAS SEPARATOR TO SRS/AES REGEN OUT
TO PUMP/ DAMPER
Pre-plumbed to Pump Pulse Damper
Backpressure Coil
14 MPa (2000 psi) at 1.0 mL/min TO EGC CO3 MIXER IN
To waste
Connect to Suppressor Regen Out
Connect to Gas Separator Assembly
Figure 5-65. Plumbing for Initial Filling of the EGC CO3 Mixer with Carbonate Eluent
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1. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) and a 10-32 to 10-32 coupler (P/N 042627) in the ICS2000 Ship Kit (P/N 064375). 2. Use the coupler to connect one end of the backpressure coil to the TO INJ VALVE IN - P/ELUENT OUT line. 3. Connect the other end of the backpressure coil to the coupler on the mixer inlet. NOTE The backpressure coil connection is temporary; it is required only during initial filling of the mixer.
4. Direct the mixer outlet to a temporary waste container, such as a beaker. 5. Verify that the suppressor is off. To avoid damaging the suppressor always turn off the suppressor before filling the mixer. The pump flow is on during filling, however, no flow reaches the suppressor.
6. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 7. From the ICS-2000 Control panel in Chromeleon or the ICS-2000 touch screen HOME page, set the pump flow rate to the rate required for the application. 8. Turn on the pump. 9. Verify that the system backpressure is between 14 and 16 MPa (2000 and 2300 psi). If necessary, adjust the pressure by adding or removing backpressure tubing. 10. From the Chromeleon Control panel or the touch screen ELUENT GENERATOR page, set the EGC-1 concentration to the value required for your application. 11. Turn on the EGC-1 current.
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12. Run at these settings until a consistent flow of eluent is exiting the mixer outlet. At a flow rate of 1 mL/min it will take about 16 minutes to fill a 4-mm mixer and about 5 minutes to fill a 2-mm mixer. NOTE The void volume of the 4-mm mixer is about 16 mL. The void volume of the 2-mm mixer is about 5 mL.
13. Turn off the EGC-1 current. 14. Turn off the pump. 15. Remove the backpressure coil from the TO INJ VALVE IN - P/ELUENT OUT line and the mixer inlet. 16. Retain the coupler on the mixer inlet. 17. Reconnect the TO INJ VALVE IN - P/ELUENT OUT line to the coupler on the mixer inlet. 18. Reconnect the mixer outlet line to port P (2) on the injection valve.
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Filling the EGC CO3 Mixer with Carbonate/Bicarbonate Eluent
Figure 5-66 illustrates the liquid flow path through the eluent generator components during initial filling of the EGC CO3 Mixer with carbonate/bicarbonate eluent. To the EluGen cartridge inlet port
EGC IN
EGC OUT
From the EluGen cartridge outlet port
EGC DEGAS
TO DEGAS ELUENT OUT
M /EP -TC OUT R C N TO EGE lue) R (b
ELUENT IN
TO DEGAS ELUENT IN
TO CR-TC/EPM ELUENT OUT (yellow)
TO EL CRUE TC (re NT /EP d) I N M
(red) (yellow)
EPM
TO EGC CO3 MIXER OUT TO CR-TC/EPM REGEN IN (orange) TO PUMP/ DAMPER
TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
BackPressure Coil*
WASTE, GAS SEPARATOR
(blue)
EGC CO3 Mixer
TO INJ VALVE PORT P TO EGC CO3 MIXER IN
TO SRS/AES REGEN OUT
Connect to Gas Separator Assembly
*14 MPa (2000 psi) at 1.0 mL/min
Figure 5-66. Plumbing for Initial Filling of the EGC CO3 Mixer with Carbonate/Bicarbonate
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1. Locate the following items in the ICS-2000 Ship Kit (P/N 064375): a yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765), a 10-32 to 10-32 coupler (P/N 042627), and a 10-32 to 1/4-28 coupler (P/N 042806). 2. Use the 10-32 to 10-32 coupler to connect one end of the backpressure coil to the TO INJ VALVE IN - P/ELUENT OUT line (see Figure 5-67). 3. Connect the other end of the backpressure coil to the coupler on the mixer inlet. 4. Use the 10-32 to 1/4-28 coupler to connect the mixer outlet to the TO SRS/AES REGEN OUT line. NOTE The backpressure coil connection is temporary; it is used only during initial filling of the mixer.
Mixer Outlet
TO SRS/AES REGEN OUT
Mixer Inlet Backpressure Coil
TO INJ PORT IN - P/ELUENT OUT
Figure 5-67. Mixer Connected Directly to Eluent Generator Outlet for Initial Filling
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5. Verify that the suppressor is off. To avoid damaging the suppressor always turn off the suppressor before filling the mixer. The pump flow is on during filling, however, no flow reaches the suppressor.
6. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 7. Set the pump flow rate to the rate required for the application. 8. Turn on the pump. 9. Verify that the system backpressure is between 14 and 16 MPa (2000 and 2300 psi). If necessary, adjust the pressure by adding or removing backpressure tubing. 10. Set the EGC-1 and EGC-2 concentrations to the values required for your application. For example, for a 3.5 mM K2CO3/1.0 mM KHCO3 mixture, set the EGC-1 concentration to 3.5 mM and the EGC-2 concentration to 1.0 mM. 11. Turn on the EGC-1 and EGC-2 currents. 12. Run at the selected settings until the mixer is filled with the eluent mixture. At a flow rate of 1 mL/min it will take about 45 minutes to fill the 4-mm mixer and about 15 minutes to fill the 2-mm mixer. NOTE The void volume of the 4-mm mixer is about 16 mL. The void volume of the 2-mm mixer is about 5 mL.
13. Turn off the EGC-1 and EGC-2 currents. 14. Turn off the pump. 15. Remove the backpressure coil from the TO INJ VALVE IN - P/ELUENT OUT line and the mixer inlet. Reconnect the two lines. 16. Disconnect the mixer outlet from the TO SRS/AES REGEN OUT line and remove the 10-32 to 1/4-28 coupler. 17. Reconnect the TO SRS/AES REGEN OUT line to the suppressor REGEN OUT port. 18. Reconnect the mixer outlet line to port P (2) on the injection valve.
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5.21 Replacing the EGC Holder and Degas Assembly 5.21.1 Disconnecting and Removing the EluGen Cartridge 1. Turn off the power to the ICS-2000. 2. Disconnect the following EGC holder liquid lines:
• •
Disconnect the line labeled TO INJ VALVE IN - P/ELUENT OUT from either port P (2) on the injection valve, or if an EGC CO3 Mixer inlet is installed, from the mixer inlet. If a CR-TC is installed, disconnect the line labeled TO SRS/AES from the REGEN OUT port on the suppressor.
REGEN OUT
• •
Disconnect the line labeled TO PUMP/DAMPER from the pump damper. Disconnect the line labeled WASTE-GAS SEPARATOR from the gas separator waste tube assembly installed on the waste container.
3. Disconnect the EluGen cartridge cable, and the CR-TC or EPM cable (if installed) from their respective connectors on the ICS-2000 top cover. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), or a corrosive acid (MSA). Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), ou un acide corrosif (MSA). Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), oder eine korrodierende Säure (MSA). Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
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4. Remove the EGC VENT line (see Figure 5-68) from the EluGen cartridge by unscrewing the luer lock from the luer adapter.
Luer Adapter Luer Lock
EGC Vent Line
If necessary, use a wrench to hold the luer adapter in place while unscrewing the vent line. Figure 5-68. EluGen Cartridge Vent Line and Luer Fitting
5. Install the luer cap (P/N 053981), provided with the EluGen cartridge, onto the luer adapter. This prevents leaks from the vent opening when you turn over the EluGen cartridge (see Step 8). 6. If an EPM is installed, lift up the bracket with the EPM attached and remove it from the EGC holder. 7. Lift the EluGen cartridge straight up and out of the EGC holder. 8. Turn the cartridge upside down and set it in the EluGen cartridge service area on top of the ICS-2000 (see Figure 5-32).
Figure 5-69. EluGen Cartridge in Service Area
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9. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the cartridge. 10. Lift the EGC holder out of the top cover and pull the liquid lines through the tubing chase (see Figure 5-70) to remove them from the ICS2000.
Tubing Chase
Figure 5-70. Top Cover Tubing Chase
11. If a CR-TC is installed, go on to Section 5.21.2. 12. If an EPM is installed, go on to Section 5.21.3. 13. If neither a CR-TC or EPM is installed, go on to Section 5.21.4.
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5.21.2 Removing the CR-TC and Reinstalling it in the New EGC Holder 1. Turn the holder upside down to view the CR-TC. 2. Grasp the top of the CRTC and lift up to disconnect it from the holder.
Disconnect liquid lines from 4 ports
3. Disconnect the liquid lines from the four ports on the CR-TC (see Figure 5-54).
Figure 5-71. Disconnecting CR-TC Liquid Lines
4. Turn the new holder upside down (see Figure 5-72) and connect the liquid lines to the CR-TC.
Couplers
NOTE To help retain the fittings and ferrules on the lines, remove the coupler from each line just before connecting the line to a port. Metal stud for mounting the CR-TC
Figure 5-72. EGC Holder (upside down)
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5. Check that none of the lines are caught under the CR-TC and then push the CR-TC onto the metal stud inside the EGC holder. Push down until the CR-TC snaps in place (see Figure 5-73).
Figure 5-73. CR-TC Installed in Holder
6. Feed the CR-TC cable through the slot on the side of the EGC holder (see Figure 5-74).
CR-TC Cable
Figure 5-74. CR-TC Cable
7. Turn the EGC holder right side up and set it on top of the ICS-2000. 8. Direct the WASTE, GAS SEPARATOR line from the top of the ICS2000 to the rear panel. Snap the line onto one of the tubing clips on the rear panel. Connect the line to the gas separator waste tube (see Section B.10.1).
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9. Feed the following liquid lines from the bottom of the holder through the tubing chase to the ICS-2000 front component panel.
• • •
TO SRS/AES REGEN OUT TO INJ VALVE IN - P/ELUENT OUT TO PUMP/DAMPER
10. Connect the lines to their respective locations:
•
Connect the line labeled TO SRS/AES REGEN OUT to the REGEN port on the suppressor.
OUT
• •
Connect the line labeled TO INJ VALVE IN - P/ELUENT OUT to port P (2) on the injection valve. Connect the line labeled TO PUMP/DAMPER to the pulse damper.
11. Go on to Section 5.21.5.
5.21.3 Removing the EPM and Reinstalling it in the New EGC Holder 1. Turn the EGC holder upside down to view the connections on the bottom of the holder. 2. Disconnect the following lines that connect from the EGC degas assembly inside the EGC holder to the EPM:
• • •
Disconnect the line labeled TO CR-TC ELUENT IN (red label) from the coupler that connects it to the line labeled TO CR-TC/EPM ELUENT IN (red label). Disconnect the line labeled TO CR-TC ELUENT OUT (yellow label) from the coupler that connects it to the line labeled TO CRTC/EPM ELUENT OUT (yellow label). Disconnect the line labeled TO CR-TC REGEN OUT (blue label) from the coupler that connects it to the line labeled TO CRTC/EPM REGEN OUT (blue label).
3. Remove the old EGC holder.
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4. Thread the three lines from the EPM (red, yellow, and blue labels) through the opening on the side of the new holder (see Figure 5-75).
TO CR-TC/EPM ELUENT IN (red label)
TO CR-TC/EPM ELUENT OUT (yellow label)
TO CR-TC/EPM REGEN OUT (blue label)
Figure 5-75. TO CR-TC/EPM Lines Outside of Holder
5. Turn the new EGC holder upside down (see Figure 5-76). NOTE To help retain the fittings and ferrules on the lines, remove the coupler from each line just before connecting the line to a port. Figure 5-76. EGC Holder (upside down)
6. Connect the lines from the EPM (red, yellow, and blue labels) to the corresponding lines in the holder. 7. Disconnect the line labeled TO CR-TC/EPM REGEN IN (orange label) from the REGEN IN port on the EPM and connect the new TO CRTC/EPM REGEN IN line (orange label) to the port.
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8. Turn the EGC holder right side up and set it in place on top of the ICS-2000. 9. Slide the EPM mounting bracket and connected EPM onto the side of the EGC holder. 10. Feed the following liquid lines through the tubing chase to the ICS2000 front component panel.
• • •
TO SRS/AES REGEN OUT TO INJ VALVE IN - P/ELUENT OUT TO PUMP/DAMPER
11. Connect the lines to their respective locations:
•
Connect the line labeled TO SRS/AES REGEN OUT to the REGEN port on the suppressor.
OUT
• •
Connect the line labeled TO INJ VALVE IN - P/ELUENT OUT to the EGC CO3 Mixer inlet. Connect the line labeled TO PUMP/DAMPER to the pulse damper.
12. Direct the WASTE, GAS SEPARATOR line from the top of the ICS2000 to the rear panel. Snap the line onto one of the tubing clips on the rear panel. Connect the line to the gas separator waste tube (see Section B.10.1). 13. Go on to Section 5.21.5.
5.21.4 Installing the New EGC Holder without a CR-TC or EPM Follow the instructions in this section if a CR-TC or EPM is not installed. 1. Set the new EGC holder in place on top of the ICS-2000. 2. Feed the following liquid lines through the tubing chase to the ICS2000 front component panel.
• • •
TO SRS/AES REGEN OUT TO INJ VALVE IN - P/ELUENT OUT TO PUMP/DAMPER
3. Connect the lines to their respective locations:
•
Connect the line labeled TO SRS/AES REGEN OUT to the REGEN port on the suppressor.
OUT
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Connect the line labeled TO INJ VALVE IN - P/ELUENT OUT to the EGC CO3 Mixer inlet. Connect the line labeled TO PUMP/DAMPER to the pulse damper.
4.
Direct the WASTE, GAS SEPARATOR line from the top of the ICS2000 to the rear panel. Snap the line onto one of the tubing clips on the rear panel. Connect the line to the gas separator waste tube (see Section B.10.1).
5.
Go on to Section 5.21.5.
5.21.5 Reinstalling the EluGen Cartridge 1. Pull the coiled black EGC IN and EGC OUT lines out from inside the EGC holder. Disconnect the EGC IN line from the coupler that connects it to the EGC OUT line. 2. Connect the EGC IN line to the EluGen cartridge INLET port (see Figure 5-77).
EGC IN INLET Port
EGC OUT OUTLET Port
3. Remove the coupler and connect the EGC OUT line to the EluGen cartridge OUTLET port.
Figure 5-77. EluGen Cartridge Inlet and Outlet Port Connections
4. Turn over the EluGen cartridge (fittings facing down). Check for any bubbles in the eluent generation chamber, and if necessary, shake and tap the EluGen cartridge to remove them. 5. Reinstall the EluGen cartridge in the holder. 6. Reconnect the EluGen cartridge cable and the CR-TC or EPM cable (if installed). 7. Remove the cap from the luer adapter on the EluGen cartridge vent opening and re-connect the EGC VENT line.
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A • Specifications
A.1
Electrical Main Power
Fuses
A.2
Two 3.15 amp fast-blow IEC 127 fuses (P/N 954745)
Physical Dimensions (without reservoir or EluGen cartridge) Weight Decibel Level
A.3
85 to 265 Vac, 47 to 63 Hz. The ICS-2000 power supply is autosensing and requires no voltage adjustment
Height: 56.1 cm (22.1 in) Width: 22.4 cm (8.8 in) Depth: 53.3 cm (21.0 in)
30 kg (66 lb) < 52 dbA
Environmental Operating Temperature
4 to 40 °C (40 to 104 °F)
Humidity
5 to 95% relative humidity, noncondensing
Operating Pressure
35 MPa (5000 psi) maximum liquid path (tubing, valve, columns, etc.)
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A.4
Front Panel Power LED
On when power is present; off when no power is present
LCD Touch Screen
¼ VGA (320 x 240 pixels) liquid crystal display with touch screen, which provides:
• • •
A.5
Display of conductivity data plot and operating status Local control of calibration and diagnostic functions
Pump Type Flow Rate
Dual-piston (in series), variable speed, 100 µL per revolution Settable range: 0.00 to 5.00 mL/min (without eluent generator) 0.10 to 3.00 mL/min (with eluent generator), in 0.01 increments Optimal Operational Range: 0.40 to 2.0 mL/min
Flow Accuracy
Save Installation). 5. If you are going to add one or more DX-LAN devices to the timebase, go on to Section B.8.2. Otherwise, exit the Server Configuration program and then go on to Section B.9.
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B.8.2
Assigning DX-LAN Devices to the Timebase (Optional) Follow the instructions in this section if you are adding one or more devices to the timebase that are connected to the PC through a DX-LAN interface (not through USB connections). 1. Follow the instructions in Installing the Chromeleon Chromatography Management System with a Dionex Ion Chromatography (IC) (Document No. 031883) to add the DX-LAN card to the server configuration as a sharable device. 2. Select the timebase that was created for the ICS-2000 (see Figure B-17); then, click the Add device icon on the toolbar (or select Edit>Add Device).
Figure B-17. Example: ICS-2000 Timebase
The Add device to timebase dialog box appears.
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Setting Up Chromeleon
3. Under Manufacturers, select Dionex: IC Modules and then select the device from the Devices list.
Figure B-18. Add Device to Timebase Dialog Box
4. Click OK. A configuration properties dialog box for the device appears. Figure B-19 shows an example of the properties for an AS50 Autosampler.
Figure B-19. AS50 Configuration Properties
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5. On the General tab page, clear the Demo Mode check box if it is currently selected, and then select the DX-LAN Device ID number. Note: Devices display their DX-LAN ID numbers when their power is turned on. 6. Click OK to close the dialog box. 7. Save the configuration (select File>Save Installation). 8. Exit the Server Configuration program. 9. Go on to Section B.9.
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Installing and Plumbing the Columns and Suppressor
B.9
Installing and Plumbing the Columns and Suppressor NOTE This section provides brief installation and plumbing instructions for the columns and suppressor. Before beginning the installation, refer to the column and suppressor manuals for detailed start-up and installation instructions. The manuals are provided on the Dionex Reference Library CD-ROM (P/N 053891).
Before beginning:
• • •
Remove the guard column, separator column, and suppressor from their boxes. Remove the fitting plugs from the ends of each column and from all ports on the suppressor. Discard any tubing temporarily connecting the suppressor ports.
B.9.1
Setting Up the Column Heater 1. Cut off the two shipping ties from the column heater and remove them (see Figure B-20). 2. Loosen the two thumbscrews on the heater cover (they remain attached to the cover).
Thumbscrew (2)
Shipping Tie (2)
3. Pull the heater cover straight out to remove it.
Figure B-20. ICS-2000 Column Heater Setup
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4. Unscrew the six thumbscrews on the top metal plate (see Figure B-21) and remove the plate.
Thumbscrew (6)
5. Go on to Section B.9.2.
Figure B-21. ICS-2000 Column Heater Cover Removed
B.9.2
Installing the Columns 1. Remove the coupler connecting GUARD IN and GUARD OUT. 2. Connect GUARD IN to the guard column inlet. Check the arrow on the column label; it should point down (flow away from the injection valve). 3. Connect GUARD OUT to the guard column outlet. 4. Push the guard column onto the back column clip. 5. Remove the coupler connecting COL IN and COL OUT. 6. Connect COL IN to the separator column inlet. Connect COL OUT to the separator column outlet. Check the arrow on the column label. It should point up (flow toward the cell). 7. Push the separator column onto the front column clips. 8. Replace the top metal plate on the column heater.
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Installing and Plumbing the Columns and Suppressor
B.9.3
Installing the Suppressor 1. Locate the suppressor mounting tabs on the component panel (see Figure B-22). Reach into the opening between the tabs and pull the yellow connector and attached cable slightly out of the opening. 2. Connect this cable to the cable from the suppressor (align the pins on the two connectors and push them together).
1 Suppressor Mounting Tabs
4
2 Suppressor Cable Connector
3
3 Guideline for AES 4 Guideline for SRS
1
1
2
1
Figure B-22. Suppressor Mounting Tabs and Guidelines
3. Orient the suppressor with the REGEN OUT fitting on top and the cable to the right. 4. Feed the cable into the opening in the component panel. 5. Align the top of the suppressor with the guideline printed on the component panel (see Figure B-22) and align the slots on the rear of the suppressor with the tabs on the panel.
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ICS-2000 Ion Chromatography System
6. Press the suppressor onto the tabs and then slide it down to lock it in place. Pull slightly on the center of the suppressor to verify that it is securely fastened. Figure B-23 shows an SRS suppressor installed on the component panel. 7. Remove the coupler connecting ELUENT IN and ELUENT OUT and connect these lines to the corresponding ports on the suppressor.
Figure B-23. Suppressor Installed (SRS Shown)
8. Remove the fitting plug from REGEN IN and connect it to the REGEN IN port on the suppressor. Do not connect the REGEN OUT port until after completing the eluent generator setup (Section B.14). 9. Replace the cover on the column heater, making sure the GUARD IN line is aligned with the slot on the side of the heater cover. 10. Go on to Section B.10.
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Connecting the Waste Lines
B.10 Connecting the Waste Lines The ICS-2000 has the following waste lines:
•
PUMP WASTE
•
TO WASTE OUT carries
•
WASTE, GAS SEPARATOR carries
carries prime waste from the pump. sample overflow from the injection valve. system waste from the suppressor.
1. Untape the coiled waste lines from the rear panel. Place the ends of the PUMP WASTE and TO WASTE OUT lines into a waste container. 2. Direct the WASTE, GAS SEPARATOR line from the top of the ICS-2000 to the rear panel. Snap the line onto one of the tubing clips on the rear panel. Connect the line to the gas separator waste tube (see Section B.10.1). NOTE To prevent waste from siphoning back into the system, check the lines periodically to be sure they are not bent, pinched, or elevated at any point.
B.10.1 Installing the Gas Separator Waste Tube 1. Locate the gas separator waste tube assembly in the ICS2000 Ship Kit (P/N 064375). 2. Connect the WASTE,
Waste, Gas Separator Line (from the suppressor)
Open to the air
GAS SEPARATOR
line from the suppressor to one of the 3-mm (1/8-in) ID white Teflon lines on the gas separator waste tube assembly (see Figure B-24).
Gas Separator Waste Tube This line is Assembly provided for a second system if needed.
Waste
Figure B-24. Gas Separator Waste Tube Installation
3. Place the gas separator waste tube assembly into the waste container. Make sure the tubing junction (where the white Teflon tubing meets the black polyethylene tubing) is above the top of the container and
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ICS-2000 Ion Chromatography System
that the gas separator waste tube and the waste container are open to the atmosphere. 4. Go on to Section B.11. DO NOT CAP THE WASTE CONTAINER: The ICS-2000, Atlas Electrolytic Suppressor, and Self-Regenerating Suppressor (SRS) use an electrolytic process that results in the production of small amounts of oxygen or hydrogen gas. To ensure that the gas is not trapped in a closed container and allowed to concentrate, install a 1.3-cm (0.52-in) ID black gas separator waste tube (P/N 045460) in an uncapped waste container. Connect the Waste, Gas Separator line to the waste tube (see Figure B-24). NE FERMEZ PAS LE CONTENEUR DE GAZ RÉSIDUEL: Le ICS-2000, le Atlas Electrolytic Suppressor, et le Self-Regenerating Suppressor (SRS) travaillent avec un proces d´électrolyse, qui produit des petites quantités de gaz d´oxygène ou d´hydrogène. Afin de garantir que le gaz ne soit pas enfermé dans un conteneur fermé et puisse s´y concentrer, connectez un tube noir à gaz résiduel (diamètre intérieur = 1,3 cm; n° de commande 045460) à un conteneur ouvert (non fermé). Connectez le conteneur résiduel au tube résiduel/gaz séparateur (désigné: « Waste, Gas Separator»). VERSCHLIESSEN SIE DEN ABFALLBEHÄLTER NICHT: Der ICS-2000, Atlas Electrolytic Suppressor und Self-Regenerating Suppressor (SRS) verwenden einen Elektrolyseprozess, wodurch kleine Mengen an Sauerstoff und Wasserstoff entstehen. Führen Sie einen schwarzen Gasabscheiderschlauch (ID = 1,3 cm; Bestell-Nr. 045460) in einen offenen (unverschlossenen) Abfallbehälter, damit sich das Gas nicht in einem geschlossenen Behälter sammelt und aufkonzentriert. Verbinden Sie die mit Waste, Gas Separator bezeichnete Leitung mit dem Abfallschlauch.
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Setting Up the Eluent Reservoir
B.11 Setting Up the Eluent Reservoir 1. Rinse the eluent reservoir. 2. Fill the reservoir with ASTM filtered, Type I (18-megohm) deionized water. 3. Place the reservoir on top of the ICS-2000. 4. Install the cap and handtighten. NOTE The ICS-2000 does not require pressurized reservoirs. However, if eluent is manually degassed or is sensitive to contamination, Dionex recommends pressurizing the reservoir with helium or nitrogen. See Section B.21 for instructions.
5. Go on to Section B.12.
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ICS-2000 Ion Chromatography System
B.12 Setting the Eluent Level After filling the reservoir, open the touch screen HOME page and enter the volume of liquid in the reservoir in the Eluent Level field (see Figure B-25), or enter the volume in the Eluent Bottle field on the Chromeleon Control panel (see Figure B-26). The ICS-2000 determines the eluent usage, by monitoring the flow rate and the length of time the pump is on, and updates the field as the eluent is used up. A warning is displayed if the level falls below 200 mL. The warning is repeated at 100 mL and at 0 mL. In order for the eluent level displayed on the screen to be accurate, the level must be entered by the user when the reservoir is filled. The ICS-2000 does not automatically detect when the reservoir is filled, nor when it is empty.
Enter the volume of liquid in the reservoir
Note: The Eluent Level field is updated as the liquid is used up.
Figure B-25. Home Page: Setting the Eluent Level
Enter the volume of liquid in the reservoir
Note: The Eluent Bottle field and slider gauge are updated as the liquid is used up.
Figure B-26. Chromeleon Control Panel: Setting the Eluent Level
Go on to Section B.13.
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Priming the Pump
B.13 Priming the Pump 1. Verify that the eluent reservoir is filled, the reservoir cap is installed and handtightened, and the liquid line from the ICS-2000 to the reservoir cap is connected (see Section B.11). 2. Verify that the waste lines are directed to a waste container. 3. The priming procedure consists of two parts:
• •
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Priming the eluent lines with a syringe (see Section B.13.1). Perform this procedure at initial installation, after changing eluents, or when eluent lines are empty. Priming the pump heads with the Prime button (see Section B.13.2). Perform this procedure after the eluent lines are primed.
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ICS-2000 Ion Chromatography System
B.13.1 Priming the Eluent Lines with a Syringe NOTE Prime the eluent lines after initial installation, after changing eluents, or when eluent lines are empty.
1. Verify that the pump is turned off. 2. Connect a 10 mL syringe (P/N 054578) to the port in the priming valve on the primary pump head (see Figure B-27).
Secondary Pump Head
Waste Valve (close) Port Primary Pump Head
10 mL Syringe (P/N 054578)
Priming Valve (open)
Figure B-27. Priming the Eluent Lines
3. Open the priming valve by turning it one-quarter to one-half turn counterclockwise. 4. On the ICS-2000 touch screen, touch the page name (for example, of pages.
B-32
) in the bottom right corner to open a menu
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Priming the Pump
5. Touch PUMP to open the touch screen PUMP page (see Figure B-28). Under Eluent Valve, touch the Open button.
Figure B-28. Pump Page: Eluent Valve Open
6. Draw the syringe back to begin pulling eluent through the flow path. It may take several syringe draws to remove all air or previous eluent from the tubing. Draw out a minimum of 20 mL of eluent to ensure that the vacuum degas assembly is primed. 7. After priming the lines thoroughly, close the priming valve. Do not overtighten the priming valve. 8. Touch Eluent Valve Closed on the touch screen PUMP page.
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ICS-2000 Ion Chromatography System
B.13.2 Priming the Pump Heads with the Prime Button NOTE Perform this procedure after priming the eluent lines (see Section B.13.1).
1. Check that the priming valve on the primary pump head is closed (see Figure B-29).
Secondary Pump Head
Waste Valve (open)
Priming Valve (close)
Primary Pump Head
Figure B-29. Priming the Pump
2. Open the waste valve on the secondary pump head by turning the knob one-quarter to one-half turn counterclockwise (see Figure B-29). Opening the valve directs the eluent flow path to waste and eliminates backpressure. 3. Touch Prime on the ICS-2000 touch screen HOME page. Confirm that the waste valve is open by pressing OK when the reminder message appears. The pump will begin pumping at approximately 3 mL/min. 4. Continue priming the ICS-2000 until no air bubbles are exiting the pump waste line. 5. Press Pump Off. 6. Close the waste valve. Do not overtighten. The pump is now ready for operation. 7. Go on to Section B.14. NOTE If the two standard priming procedures described above are unsuccessful, prime the pump with isopropyl alcohol. See Section 5.15 for instructions.
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Setting Up the Eluent Generator
B.14 Setting Up the Eluent Generator Before Beginning
Remove the EluGen cartridge (EGC) and the other items to be installed from their shipping containers. Depending on the type of eluent to be generated, the other items may include a Continuously Regenerated Trap Column (CR-TC), an EPM Electrolytic pH Modifier, and/or an EGC CO3 Mixer. NOTE The EGC degas assembly is installed inside the EGC holder at the factory. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution concentrée de K2CO3. Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), eine korrodierende Säure (MSA) oder eine konzentrierte K2CO3-Lösung. Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
Refer to the EluGen cartridge, CR-TC, and EPM manuals for the optimal operating conditions for your application. The manuals are provided on the Dionex Reference Library CD-ROM (P/N 053891).
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ICS-2000 Ion Chromatography System
B.14.1 Eluent Generator Setup for KOH, LiOH, MSA, and NaOH Eluents Follow the instructions in this section if you are installing a KOH, LiOH, MSA, or NaOH EluGen cartridge and a CR-TC.
• •
If you are installing a K2CO3 cartridge, an EPM, and an EGC CO3 Mixer (for generating carbonate/bicarbonate eluent), go to Section B.14.2. If you are installing a K2CO3 cartridge and an EGC CO3 Mixer (for generating carbonate eluent), go to Section B.14.3.
Overview
The eluent generator setup procedure for KOH, LiOH, MSA, or NaOH eluents consists of the following main steps:
B-36
•
Installing the CR-TC.
•
Installing the EluGen cartridge.
•
Connecting the EluGen cartridge vent line.
•
Recording the EluGen cartridge serial number in Chromeleon.
•
Conditioning the EluGen cartridge.
•
Hydrating the CR-TC.
•
Completing the eluent generator setup.
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Setting Up the Eluent Generator
Items Required to Complete the Setup Procedure
In addition to the EluGen cartridge and the CR-TC, you will need the following items to complete the eluent generator setup.
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Item
P/N
Use To
Yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (supplied in the ICS-2000 Ship Kit (P/N 064375))
053765
Provide backpressure during setup procedures.
EluGen Cartridge Vent Line Tubing Kit (supplied with the cartridge)
063092
Vent the cartridge during operation.
10-32 to 1/4-28 coupler (supplied in the ICS-2000 Ship Kit)
042806
Temporary connection during setup procedures.
Temporary waste container (beaker, bottle, etc.) (not supplied)
n/a
Collect waste during setup procedures.
10-32 fittings 10-32 ferrules
043275 043276
Complete the connections
1/8-in fittings 1/8-in ferrules
052267 048949
Complete the connections
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ICS-2000 Ion Chromatography System
Figure B-30 illustrates the ICS-2000 after the EluGen cartridge is installed.
IN
EGC OUT
EluGen Cartridge (EGC) EGC Holder
EGC and CR-TC Cable Connections
Figure B-30. ICS-2000 with an EluGen Cartridge Installed (Top View)
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Setting Up the Eluent Generator
Figure B-31 illustrates the liquid flow path through the eluent generator components after all setup steps are complete and the eluent generator is ready for operation.
EGC VENT
EGC II KOH, LiOH, MSA, or NaOH
Send to waste
Inlet
Outlet
EGC IN
EGC OUT
TO DEGAS ELUENT OUT
EGC DEGAS CR-TC
Eluent Out
Regen Out Eluent In
TO DEGAS ELUENT IN
Regen In
TO CR-TC ELUENT IN (red)
TO CR-TC REGEN OUT TO (blue) RE C R (o GE -TC ra N ng IN e)
TO CR-TC/EPM ELUENT OUT (yellow)
DEGAS ELUENT OUT
Backpressure Coil* TO PUMP/ DAMPER
TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
Connect to Inject Valve Port P (2)
*Add backpressure coils, if needed, to create a system backpressure of between 14 and 16 MPa (2000 and 2300 psi).
WASTE, GAS SEPARATOR TO SRS/AES REGEN OUT
Connect to Connect to Suppressor Gas Separator Regen Out Assembly
Figure B-31. Eluent Generator Flow Schematic with CR-TC: Use for Generating KOH, LiOH, MSA, or NaOH Eluent
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ICS-2000 Ion Chromatography System
Installing the CR-TC
1. Tilt the cartridge holder to view the bottom of the holder and brace the holder against the back corner of the ICS-2000 (see Figure B-32).
Metal ball stud for mounting the CR-TC
Figure B-32. Cartridge Holder (tilted to view the bottom)
2. Before installing the CR-TC, note the metal ball stud inside the bottom of the cartridge holder (see Figure B-32) and the bracket on the CR-TC mounting plate (see Figure B-33). These are used to mount the CR-TC inside the holder after it is plumbed.
E= Electrical connection (2) (Do not remove) P=Port (4) (Remove plugs)
E
P P
P E
P
Bracket for mounting the CR-TC on the holder
Figure B-33. CR-TC
3. Remove the plugs from the four ports, labeled “P” in Figure B-33. Do not remove the two electrical connections, labeled “E” in the figure.
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Setting Up the Eluent Generator
4. With the CR-TC oriented as shown in Figure B-34, connect each line to the corresponding port on the CR-TC. NOTE To help retain the fittings and ferrules on the lines, remove the coupler from each line just before connecting the line to a port.
Regen Out Eluent Out
Eluent In
Regen In
Figure B-34. Plumbed CR-TC
5. Check that none of the lines are caught under the CR-TC and then push the CR-TC onto the metal stud inside the EGC holder (see Figure B-35). Push down until the CR-TC snaps into place.
Figure B-35. CR-TC Installed in Holder
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ICS-2000 Ion Chromatography System
6. Feed the CR-TC cable through the slot on the side of the EGC holder (see Figure B-36).
CR-TC Cable
Figure B-36. Installing the CR-TC
7. Turn the EGC holder right-side up and set it back into position. Installing the EluGen Cartridge
1. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the EluGen cartridge INLET and OUTLET ports (see Figure B-37).
OUTLET
INLET
Figure B-37. EluGen Cartridge Inlet and Outlet Ports
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Setting Up the Eluent Generator
2. Set the EluGen cartridge in the service area on top of the ICS-2000 and orient it with the cable toward the EGC holder (see Figure B-38).
EGC Cable
Figure B-38. EluGen Cartridge in Service Area
3. Pull the coiled black EGC IN and EGC OUT lines out slightly from the cartridge holder. 4. Disconnect the EGC IN line from the union that connects it to the EGC OUT line.
EGC IN INLET Port
5. Connect EGC IN to the EGC INLET port (see Figure B-39).
Figure B-39. EGC Inlet Port Connections
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ICS-2000 Ion Chromatography System
6.
7.
Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) in the ICS-2000 Ship Kit (P/N 064375).
Backpressure Coil
Connect one end of this coil to the EGC OUTLET port (see Figure B-40). Leave the other end of the coil unconnected.
OUTLET Port
Figure B-40. EGC Outlet Connection for Conditioning the EGC NOTE The backpressure coil connection is temporary; it is required only during the EluGen cartridge conditioning procedure described in “Conditioning the EluGen Cartridge” on page B-48.
8.
Turn the EluGen cartridge over (with the fittings facing down). Shake the EluGen cartridge vigorously, and tap it with the palm of your hand 10 to 15 times. Check that all bubbles trapped in the eluent generation chamber are dislodged.
The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution concentrée de K2CO3. Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), eine korrodierende Säure (MSA) oder eine konzentrierte K2CO3-Lösung. Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
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Setting Up the Eluent Generator
9.
Slide the EluGen cartridge down into the holder until it stops. Make sure the cable and backpressure coil remain out of the holder (see Figure B-41).
NOTE To avoid crimping the lines inside the holder, do not twist the cartridge when you slide it into the holder. The lines are designed to coil inside the holder.
Figure B-41. Installing the EluGen Cartridge in the Holder
10. Remove the plug from the EGC-1 connector on top of the ICS-2000. 11. Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure B-42. Push it onto the EGC-1 connector on the ICS2000. Twist the ring on the cable connector fingertight to secure it.
Figure B-42. Connecting the EluGen Cartridge Cable
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ICS-2000 Ion Chromatography System
Connecting the Vent Line
1. Locate the vent line tubing kit (P/N 063092) supplied with the EluGen cartridge. Slide the label onto one end of the tubing and then push the barbed luer lock onto the tubing. 2. Unscrew and remove the plug from the vent opening on the side of the EluGen cartridge (see Figure B-43).
Vent Plug (remove)
Figure B-43. EluGen Cartridge Vent Plug
3. Screw the luer adapter onto the vent opening. Remove the cap on the luer adapter by twisting. Save the cap.
Luer Adapter
Luer Lock
EGC Vent Line
4. Twist the luer lock and EluGen cartridge vent line into the luer adapter (see Figure B-44). Figure B-44. Installing the EluGen Cartridge Vent Line NOTE To prevent leaks from the EluGen cartridge, always replace the luer adapter cap before moving the EluGen cartridge.
5. Direct the EluGen cartridge vent line to the rear of the ICS-2000 and snap it onto one of the tubing clips on the rear panel. 6. Direct the vent line to the waste container and insert it down into the gas separator waste tube about 10 to 15 cm (4 to 6 in).
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Setting Up the Eluent Generator
Recording the EluGen Cartridge Serial Number in Chromeleon
The serial number is printed on the EluGen cartridge label. 1. Open the Chromeleon Server Configuration program (select Start > Programs (or All Programs) > Chromeleon > Server Configuration). 2. Double-click the ICS-2000 system icon. The properties dialog box for the ICS-2000 appears. 3. Click the Eluent Generator tab (see Figure B-45). 4. Select the EGC-1 check box and enter the EluGen cartridge serial number. 5. Click OK.
Figure B-45. Eluent Generator Configuration Properties Example
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ICS-2000 Ion Chromatography System
Conditioning the EluGen Cartridge
After completing the installation steps described in the previous sections, condition the EluGen cartridge for 30 minutes. 1. Set a temporary waste container, such as a beaker, on top of the ICS-2000 and direct the yellow backpressure coil from the EluGen cartridge OUTLET port to the container. 2. On the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min. 3. Touch the EGC button on the HOME page to open the ELUENT GENERATOR page. Set the EGC concentration to 50 mM. 4. Verify that the suppressor and CR-TC are off. To avoid damaging the suppressor and CR-TC, always turn off the suppressor and CR-TC before conditioning the EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor or CR-TC.
5. Verify that the Automatically turn on with pump options are not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9) and ELUENT GENERATOR page (see Section C.8). Disabling these options lets you turn on the pump, without automatically turning on the suppressor and CR-TC. 6. Verify that the eluent reservoir is filled with ASTM filtered, Type 1 (18 megohm-cm) deionized water (see Section B.11). 7. Turn on the pump. 8. Turn on the EluGen cartridge. 9. Run at the selected settings (1.00 mL/min at 50 mM) for 30 minutes. 10. Turn off the EluGen cartridge. 11. Turn off the pump. 12. Disconnect the EluGen cartridge cable. 13. Remove the backpressure tubing from the waste container and remove the waste container. 14. Lift the EluGen cartridge out of the holder, turn it over, and set it in the service area.
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Setting Up the Eluent Generator
15. Disconnect the backpressure coil from the EluGen cartridge OUTLET port. 16. Connect the EGC OUT line to the OUTLET port (see Figure B-46).
Figure B-46. EGC Inlet and Outlet Connections
17. Turn over the EluGen cartridge. Check for bubbles; if necessary, shake and tap the EluGen cartridge to remove bubbles. 18. Reinstall the EluGen cartridge in the holder. 19. Do not reconnect the EluGen cartridge cable until after hydrating the CR-TC. Hydrating the CR-TC
Always hydrate the CR-TC before initial operation. This requires running ASTM filtered, Type 1 (18 megohm-cm) deionized water through the CRTC for 10 minutes, while bypassing the columns and suppressor. Figure B-47 illustrates the liquid flow path through the CR-TC during the hydration procedure.
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ICS-2000 Ion Chromatography System
Deionized water in from pump TO EGC OUT
TO DEGAS ELUENT OUT
EGC DEGAS CR-TC
Eluent Out
Regen Out Eluent In
TO DEGAS ELUENT IN
Regen In
TO CR-TC ELUENT IN (red)
TO CR-TC REGEN OUT TO (blue) RE C R (o GE -TC ra N ng IN e)
TO CR-TC/EPM ELUENT OUT (yellow)
DEGAS ELUENT OUT
WASTE, GAS SEPARATOR
10-32 to 1/4-28 Coupler TO INJ VALVE IN - P/ ELUENT OUT
TO SRS/AES REGEN OUT
Figure B-47. CR-TC Plumbing for Hydration
1. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from port P (2) on the injection valve. 2. Disconnect the TO SRS/AES REGEN OUT line from the suppressor. 3. Use a 10-32 to 1/4-28 coupler (P/N 042806) to connect the TO INJ VALVE IN - P/ELUENT OUT line to the SRS/AES REGEN OUT line. 4. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before hydrating the CR-TC. The pump flow is on during conditioning, however, no flow reaches the suppressor.
5. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor.
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Setting Up the Eluent Generator
6. Turn on the pump and set the flow to the rate recommended for your application. 7. Pump deionized water through the CR-TC for at least 10 minutes. 8. Turn off the pump and remove the coupler. Completing the Eluent Generator Setup
1. Reconnect the TO SRS/AES REGEN OUT line to the REGEN OUT port on the suppressor. 2. Reconnect the TO INJ VALVE IN - P/ELUENT OUT line to port P (2) on the injection valve. 3. Reconnect the EluGen cartridge cable. 4. Remove the plug from the CR-TC connector on top of the ICS-2000 5. Orient the CR-TC’s black 3-pin electrical cable connector as shown in Figure B-42. Push it onto the CR-TC connector on the ICS2000. Twist the ring on the cable connector and fingertighten to secure it. Figure B-48. Connecting the CR-TC Cable NOTE Backpressure tubing may be required between the injection valve and the EGC degas eluent outlet. The EluGen cartridge requires 14 to 16 MPa (2000 to 2300 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. See Section B.16.1 for details.
Go on to Section B.15.
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ICS-2000 Ion Chromatography System
B.14.2 Eluent Generator Setup for Carbonate/Bicarbonate Eluent Follow the instructions in this section if you are installing a K2CO3 cartridge, an EPM, and an EGC CO3 Mixer (for generating carbonate/bicarbonate eluent).
• •
If you are installing a K2CO3 cartridge and an EGC CO3 Mixer (for generating carbonate eluent), go to Section B.14.3. If you are installing a KOH, LiOH, MSA, or NaOH EluGen cartridge and a CR-TC, go to Section B.14.1.
Overview
The eluent generator setup procedure for carbonate/bicarbonate eluent consists of the following main steps:
•
Installing the EluGen cartridge.
•
Connecting the EluGen cartridge vent line.
•
Installing the EPM.
•
Plumbing the EPM for conditioning.
•
B-52
Recording the EluGen cartridge and the EPM serial numbers in Chromeleon.
•
Conditioning the EluGen cartridge and the EPM.
•
Installing the EGC CO3 Mixer.
•
Temporarily filling the EGC CO3 Mixer with deionized water.
•
Filling the EGC CO3 Mixer with eluent of the required concentration.
•
Completing the eluent generator setup.
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Setting Up the Eluent Generator
Items Required to Complete the Setup Procedure
The following items are required to setup the EluGen cartridge, EPM, and EGC CO3 Mixer. Except as noted, all items are supplied in the ICS-2000 Ship Kit (P/N 064375). Item
P/N
Used To
EPM mounting bracket
063624
Mount the EPM on the EGC holder
35 cm (14 in) of black 0.25-mm (0.010-in) ID PEEK tubing
064340
Lengthen the line between the EGC degas eluent inlet and the EPM ELUENT OUT port
30 cm (12 in) of black 0.25-mm (0.010-in) ID PEEK tubing
064334
Lengthen the line between the EluGen cartridge outlet and the EPM ELUENT IN port
28 cm (11 in) of clear 1.58-mm (0.062-in) ID Teflon tubing
064337
Lengthen the line between the EGC degas regenerant inlet and the EPM REGEN OUT port
EluGen Cartridge Vent Line Tubing Kit (supplied with the cartridge)
063092
Vent the cartridge during operation
Yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil
053765
Provide backpressure during setup procedures
EGC CO3 Mixer mounting clips
063642
Install the mixer
Phillips head screwdriver (not supplied)
n/a
Install the EGC CO3 Mixer mounting clips
35 cm (14 in) of black 0.25-mm (0.010-in) ID PEEK tubing
064346
Connect the EGC degas eluent outlet and the EGC CO3 Mixer inlet
60 cm (24 in) of black 0.25-mm (0.010-in) ID PEEK tubing
064343
Connect the EGC CO3 Mixer outlet to port P (2) on the injection valve
Temporary waste container (beaker, bottle, etc.) (not supplied)
n/a
Collect waste during setup procedures
10-32 to 10-32 coupler 10-32 to 1/4-28 coupler
042627 042806
Complete the connections
10-32 fittings 10-32 ferrules
043275 043276
Complete the connections
1/8-in fittings 1/8-in ferrules
052267 048949
Complete the connections
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B-53
ICS-2000 Ion Chromatography System
Figure B-49 illustrates the EluGen cartridge and EPM after installation.
EluGen Cartridge (EGC
EPM
EGC Holder
Figure B-49. ICS-2000 with an EluGen Cartridge and EPM Installed
B-54
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Setting Up the Eluent Generator
Figure B-50 illustrates the liquid flow path through the eluent generator components after all setup steps are complete and the eluent generator is ready for operation.
EGC VENT
EGC II K2CO3
Send to waste
Inlet
Outlet
EGC IN
EGC OUT
TO CR-TC/EPM ELUENT OUT (yellow label)
(yellow label)
TO DEGAS ELUENT OUT
EGC DEGAS
M / EP -TC UT CR EN O el) TO EG lab R lue (b
ELUENT IN
TO DEGAS ELUENT IN
TO EL C R (re UE TC/ d N T EP la be IN M l)
(red label)
EPM
TO EGC CO3 MIXER OUT TO CR-TC/EPM REGEN IN (orange label) TO PUMP/ DAMPER
EGC CO3 Mixer TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
WASTE, GAS SEPARATOR
(blue label)
Backpressure Coil*
TO EGC CO3 MIXER IN
*Add backpressure coils, as needed, to create a system backpressure of between 14 and 16 MPa (2000 and 2300 psi).
TO INJ VALVE PORT P
Connect to Inject Valve Port P (2)
TO SRS/AES REGEN OUT
Connect to Gas Separator Assembly
Connect to Suppressor Regen Out
Figure B-50. Eluent Generator Flow Schematic with an EPM and EGC CO3 Mixer: Use for Generating Carbonate/Bicarbonate Eluent
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B-55
ICS-2000 Ion Chromatography System
Installing the EluGen Cartridge
1. Tilt the cartridge holder to view the bottom and brace the holder against the back corner of the ICS-2000 (see Figure B-51).
Figure B-51. Cartridge Holder (tilted to view the bottom)
B-56
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Setting Up the Eluent Generator
2. Use the precut tubing assemblies included in the ICS-2000 Ship Kit to extend the length of three lines as described below: a. Disconnect the TO CR-TC ELUENT IN line (red label) from the coupler that connects it to the TO CR-TC ELUENT OUT line (yellow label). Connect a 32 to 10-32 coupler to the end of the TO CR-TC ELUENT IN line and connect the 30 cm (12 in) length of black PEEK tubing (red labels) (P/N 064334) to the coupler (see Figure B-63). b. Connect the 35 cm (14 in) length of black PEEK tubing (yellow labels) (P/N 064340) to the coupler on the TO CR-TC ELUENT OUT line (yellow label). c. Disconnect the TO CR-TC REGEN IN line (orange label) from the coupler that connects it to the TO CR-TC REGEN OUT line (blue label). Connect the 28 cm (11 in) length of clear Teflon tubing (blue labels) (P/N 064337) to the coupler on the TO CR-TC REGEN OUT line (blue label).
TO CR-TC/EPM ELUENT OUT Line (yellow label)
TO CR-TC/EPM ELUENT IN Line (red label)
TO CR-TC/EPM REGEN OUT Line (blue label)
Figure B-52. EPM Eluent and Regen Line Extensions
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B-57
ICS-2000 Ion Chromatography System
3.
Pull the TO CR-TC REGEN IN line (orange label) out of the opening on the side of the holder.
4.
Thread the three extended lines (red, yellow, and blue labels) through the opening on the side of the holder (see Figure B-53).
TO CR-TC/EPM ELUENT IN (red label)
TO CR-TC/EPM ELUENT OUT (yellow label)
TO CR-TC/EPM REGEN OUT (blue label)
Figure B-53. TO CR-TC/EPM Lines Outside of Holder
5. Turn the EGC holder right-side up and set it back into position. 6. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the cartridge INLET and OUTLET fittings (see Figure B-54).
OUTLET
INLET
Figure B-54. EluGen Cartridge Fitting Plugs
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Setting Up the Eluent Generator
7. Set the EluGen cartridge in the service area on top of the ICS-2000 and orient it with the cable toward the EGC holder (see Figure B-55).
EGC Cable
Figure B-55. EluGen Cartridge in Service Area
8. Pull the coiled black EGC IN and EGC OUT lines out from inside the EGC holder. Disconnect the EGC IN line from the coupler that connects it to the EGC OUT line. 9. Connect the EGC IN line to the EluGen cartridge INLET port (see Figure B-80). 10. Remove the coupler and connect the EGC OUT line to the EluGen cartridge OUTLET port.
Figure B-56. EluGen Cartridge Inlet and Outlet Port Connections
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B-59
ICS-2000 Ion Chromatography System
11. Turn the EluGen cartridge over (with the fittings facing down). Shake the EluGen cartridge vigorously, and tap it with the palm of your hand 10 to 15 times. Check that all bubbles trapped in the eluent generation chamber are dislodged. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution concentrée de K2CO3. Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), eine korrodierende Säure (MSA) oder eine konzentrierte K2CO3-Lösung. Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
12. Slide the EluGen cartridge down into the holder until it stops (see Figure B-57). Make sure the cable remains out of the holder.
NOTE To avoid crimping the lines, do not twist the cartridge when you slide it into the holder. The lines are designed to coil inside the holder.
Figure B-57. EluGen Cartridge Installed in the Holder
B-60
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Setting Up the Eluent Generator
13. Remove the plug from the EGC-1 connector on top of the ICS-2000. 14. Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure B-58. Push it onto the EGC-1 connector on the ICS2000. Twist the ring on the cable connector fingertight to secure it.
Figure B-58. Connecting the EluGen Cartridge Cable Connecting the EluGen Cartridge Vent Line
1. Locate the EluGen Cartridge Vent Line Tubing Kit supplied with the EluGen cartridge. 2. Slide the label onto one end of the tubing and then push the barbed luer lock onto the tubing. 3. Unscrew and remove the plug from the vent opening on the side of the EluGen cartridge (see Figure B-59).
Vent Plug (remove)
Figure B-59. EluGen Cartridge Vent Plug
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B-61
ICS-2000 Ion Chromatography System
4. Screw the luer adapter onto the vent opening. Remove the cap on the luer adapter by twisting. Save the cap.
Luer Adapter
Luer Lock
EGC Vent Line
5. Twist the luer lock and EluGen cartridge vent line into the luer adapter (see Figure B-60). Figure B-60. Installing the EluGen Cartridge Vent Line NOTE To prevent leaks from the EluGen cartridge, always replace the luer adapter cap before moving the EluGen cartridge.
6. Direct the vent line to the waste container and insert it down into the gas separator waste tube about 10 to 15 cm (4 to 6 in). Installing the EPM
1. Remove the plugs from the EPM eluent and regen liquid ports. 2. Push the EPM onto the ball studs on the mounting bracket (see Figure B-61).
EPM
Mounting Bracket EGC Cable
Ball Studs
Figure B-61. EPM and Mounting Bracket
B-62
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Setting Up the Eluent Generator
3. Lift the EluGen cartridge up slightly from the EGC holder and slide the EPM bracket onto the side of the holder (see Figure B-62).
EGC Cable
Figure B-62. EPM and Mounting Bracket Installed on EGC Holder
4. Connect the following lines to the EPM:
• • • •
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Connect the TO CR-TC/EPM ELUENT OUT line (yellow label) to the ELUENT OUT port on the EPM (see Figure B-63). Connect the TO CR-TC/EPM ELUENT IN line (red label) to the ELUENT IN port on the EPM. Connect the TO CR-TC/EPM REGEN IN line (orange label) to the REGEN IN port on the EPM. Connect the TO CR-TC/EPM REGEN OUT line (blue label) to the REGEN OUT port on the EPM.
B-63
ICS-2000 Ion Chromatography System
EGC VENT
EGC II K2CO3
Send to waste
Outlet 35 cm (14 in) of black
Inlet EGC IN
EGC OUT
30 cm (12 in) of black 0.25-mm (0.010-in) ID PEEK tubing (P/N 064334)
0.25-mm (0.010-in) ID PEEK tubing (P/N 064340)
(yellow label)
TO DEGAS ELUENT OUT
EGC DEGAS
M /E P -TC UT CR EN O el) TO EG lab R l ue (b
EPM
TO CR-TC/EPM REGEN IN (orange label)
28 cm (11 in) of clear 1.58-mm (0.062-in) ID Teflon tubing (P/N 064337)
TO PUMP/ DAMPER
ELUENT IN
TO DEGAS ELUENT IN
TO CR-TC/EPM ELUENT OUT (yellow label)
TO EL CR(re UE TC/ d NT EP la IN M be l)
(red label)
WASTE, GAS SEPARATOR
(blue label)
TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed Pre-plumbed to Pump Pulse to Inject Valve Damper Port P
TO SRS/AES REGEN OUT
Connect to Gas Separator Assembly
Figure B-63. EluGen Cartridge and EPM Plumbing with Tubing Extensions
5. Remove the plug from the EGC-2 connector on top of the ICS-2000. 6. Connect the EPM electrical cable to the EGC-2 connector.
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Setting Up the Eluent Generator
Recording the EluGen Cartridge and EPM Serial Numbers in Chromeleon
The serial numbers are printed on labels on the EluGen cartridge and EPM. 1. Open the Server Configuration program (select Start > Programs (or All Programs) > Chromeleon > Server Configuration). 2. Double-click the ICS-2000 system icon. The properties dialog box for the ICS-2000 appears. 3. Click the Eluent Generator tab (see Figure B-45). 4. Select the EGC-1 check box and enter the EluGen cartridge serial number. 5. Select the EGC-2 check box and enter the serial number of the EPM. 6. Click OK.
Figure B-64. Eluent Generator Configuration Properties Example
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B-65
ICS-2000 Ion Chromatography System
Plumbing the EluGen Cartridge and EPM for Conditioning
Figure B-65 illustrates the liquid flow path through the EluGen cartridge and EPM during the conditioning procedure.
EGC VENT
EGC II K2CO3
Send to waste
Inlet EGC IN
Outlet EGC OUT
TO CR-TC/EPM ELUENT OUT (yellow label)
(yellow label)
TO DEGAS ELUENT OUT
EGC DEGAS
M /EP -TC UT CR EN O el) TO EG lab R lue (b
ELUENT IN
TO DEGAS ELUENT IN
TO EL C R (re UE TC/ d N T EP lab IN M el )
(red label)
EPM
TO CR-TC/EPM REGEN IN (orange)
14 MPa (2000 psi) at 1.0 mL/min
TO PUMP/ DAMPER TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
Backpressure Coil
WASTE, GAS SEPARATOR
(blue label)
10-32 to 1/4-28 Coupler
TO SRS/AES REGEN OUT
Connect to Gas Separator Assembly
Figure B-65. EluGen Cartridge and EPM Plumbing for Conditioning with Carbonate/Bicarbonate Eluent
B-66
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Setting Up the Eluent Generator
1. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from port P (2) on the injection valve. 2. Use a 10-32 to 10-32 coupler (P/N 042627) to connect the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) to the TO INJ VALVE IN - P/ELUENT OUT line. 3. Connect a 10-32 to 1/4-28 coupler (P/N 042806) to the free end of the backpressure coil. 4. Disconnect the TO SRS/AES REGEN OUT line from the suppressor REGEN OUT port. 5. Connect the TO SRS/AES REGEN OUT line to the 10-32 to 1/4-28 coupler (see Figure B-66). NOTE The backpressure coil connection in Figure B-66 is temporary; it is required only during the EPM and EluGen cartridge conditioning procedure described in the next section.
TO SRS/AES REGEN OUT 10-32 to 1/4-28 Coupler
TO INJ VALVE IN - P/ ELUENT OUT
Backpressure Coil
10-32 to 10-32 Coupler
Figure B-66. Backpressure Coil Connections for Conditioning the EluGen Cartridge and EPM with Carbonate/Bicarbonate Eluent
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ICS-2000 Ion Chromatography System
Conditioning the EPM and EluGen Cartridge
After completing the plumbing connections described in the previous sections, follow the steps below to hydrate the EPM for 5 minutes and then condition the EPM and EluGen cartridge for 30 minutes. 1. Make sure the eluent reservoir is filled with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before conditioning the EPM and EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor.
3. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 4. On the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min. 5. Turn on the pump. 6. Run the pump for 5 minutes to hydrate the EPM. 7. Touch the EGC button on the HOME page to open the ELUENT GENERATOR page. 8. Verify that the cartridge type for EGC-1 is Carb and the type for EGC-2 is pH Mod. If the cartridge types are wrong, make sure the cartridge serial numbers were entered correctly in the Chromeleon Server Configuration program (see “Recording the EluGen Cartridge and EPM Serial Numbers in Chromeleon” on page B-65). 9. Select the following settings:
•
Set the EGC-1 concentration to 9 mM.
•
Set the EGC-2 concentration to 1 mM.
10. Turn on the EGC-1 and EGC-2 currents. 11. Run the EluGen cartridge and EPM at these settings for 30 minutes.
B-68
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Setting Up the Eluent Generator
12. Turn off the EGC-1 and EGC-2 current. 13. Turn off the pump. Installing the EGC CO3 Mixer
Figure B-67 illustrates the EGC CO3 Mixer after installation.
TO EGC CO3 MIXER OUT (P/N 064343)
TO EGC CO3 MIXER IN (P/N 064346)
Figure B-67. ICS-2000 with an EGC CO3 Mixer Installed
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B-69
ICS-2000 Ion Chromatography System
1. Use a Phillips head screwdriver to remove the existing small diameter mounting clips from the inside of the ICS-2000 door. 2. Install the larger diameter clips (P/N 063642) (see Figure B-68). Mixer Mounting Clips
Figure B-68. Location of Mounting Clips for the EGC CO3 Mixer
3. Orient the mixer with the outlet pointing upward and push it onto the clips (see Figure B-69). The mixer outlet must point upward to ensure thorough mixing of the eluent.
Mixer Outlet
4. Locate the 35 cm (14 in) length of black PEEK tubing (white labels) (P/N 064346). Connect the end labeled TO EGC CO3 MIXER IN to the mixer inlet. 5. Locate the 60 cm (24 in) length of black PEEK tubing (white labels) (P/N 064343). Connect the end labeled TO EGC CO3 MIXER OUT to the mixer outlet.
Mixer Inlet
Figure B-69. EGC CO3 Mixer Installed on the ICS-2000 Door
B-70
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Setting Up the Eluent Generator
Filling the EGC CO3 Mixer with Deionized Water
1. Verify that the EGC-1 and EGC-2 currents are off. 2. Disconnect the EluGen cartridge inlet line (labeled TO PUMP/DAMPER) from the coupler that connects it to the green pump outlet line (see Figure B-70).
TO PUMP/ DAMPER (disconnect this line)
Pump Outlet (green tubing)
Figure B-70. EluGen Cartridge Inlet and Pump Outlet
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ICS-2000 Ion Chromatography System
3. Connect the pump outlet to the mixer inlet (see Figure B-71).
Pump Outlet
Mixer Inlet
Figure B-71. Pump Outlet Connected to Mixer Inlet for Mixer Hydration
4. Direct the mixer outlet line to a temporary waste container, such as a beaker. 5. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before filling the mixer. The pump flow is on during filling, however, no flow reaches the suppressor.
6. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 7. Set the pump flow rate to 5.00 mL/min. 8. Turn on the pump. 9. Run the pump until the mixer is filled and there is a consistent flow of water exiting the mixer outlet. It takes about 5 minutes to fill a 4-mm mixer and about 2 minutes to fill a 2-mm mixer. 10. Turn off the pump.
B-72
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Setting Up the Eluent Generator
Filling the EGC CO3 Mixer with the Carbonate/Bicarbonate Eluent
Before initial use, follow the steps in this section to fill the EGC CO3 Mixer with the carbonate/bicarbonate eluent concentration required for the application to be run. Figure B-72 illustrates the liquid flow path through the eluent generator components during initial filling of the EGC CO3 Mixer with carbonate/bicarbonate eluent. EGC VENT
EGC II K2CO3
Send to waste
Inlet EGC IN
Outlet EGC OUT
EGC DEGAS
TO DEGAS ELUENT OUT
M /EP -TC UT CR EN O ) TO EG lue R (b
ELUENT IN
TO DEGAS ELUENT IN
TO CR-TC/EPM ELUENT OUT (yellow)
TO EL CRUE TC (re NT /EP d) I N M
(red) (yellow)
EPM
TO EGC CO3 MIXER OUT TO CR-TC/EPM REGEN IN (orange) TO PUMP/ DAMPER
TO INJ VALVE IN - P/ ELUENT OUT
Pre-plumbed to Pump Pulse Damper
BackPressure Coil*
WASTE, GAS SEPARATOR
(blue)
EGC CO3 Mixer
TO INJ VALVE PORT P TO EGC CO3 MIXER IN
TO SRS/AES REGEN OUT
Connect to Gas Separator Assembly
*14 MPa (2000 psi) at 1.0 mL/min
Figure B-72. EluGen Cartridge and EPM Plumbing for Initial Filling of the EGC CO3 Mixer with Carbonate/Bicarbonate Eluent
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B-73
ICS-2000 Ion Chromatography System
1. Disconnect the pump outlet from the mixer inlet. 2. Reconnect the pump outlet and the EluGen cartridge inlet. 3. Connect a 10-32 to 10-32 coupler to the mixer inlet. 4. Disconnect the outlet of the yellow PEEK backpressure coil from the TO SRS/AES REGEN OUT line and then connect the backpressure coil to the mixer inlet (see Figure B-73). 5. Connect the mixer outlet to the TO SRS/AES REGEN OUT line. NOTE The backpressure coil connection is temporary; it is required only during initial filling of the mixer.
Mixer Outlet
TO SRS/AES REGEN OUT
Mixer Inlet Backpressure Coil
TO INJ PORT IN - P/ELUENT OUT
Figure B-73. Mixer Connected Directly to Eluent Generator Outlet for Initial Filling
6. Verify that the suppressor is off.
B-74
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Setting Up the Eluent Generator
To avoid damaging the suppressor, always turn off the suppressor before filling the mixer. The pump flow is on during filling, however, no flow reaches the suppressor.
7. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 8. Set the pump flow rate to the rate required for the application. 9. Turn on the pump. 10. Verify that the system backpressure is between 14 and 16 MPa (2000 and 2300 psi). If necessary, adjust the pressure by adding or removing backpressure tubing. 11. Set the EGC-1 and EGC-2 concentrations to the values required for your application. For example, for a 3.5 mM K2CO3/1.0 mM KHCO3 mixture, set the EGC-1 concentration to 3.5 mM and the EGC-2 concentration to 1.0 mM. 12. Turn on the EGC-1 and EGC-2 currents. 13. Run at the selected settings until the mixer is filled with the eluent mixture. At a flow rate of 1 mL/min it will take about 45 minutes to fill the 4-mm mixer and about 15 minutes to fill the 2-mm mixer. NOTE The void volume of the 4-mm mixer is about 16 mL. The void volume of the 2-mm mixer is about 5 mL.
14. Turn off the EGC-1 and EGC-2 currents. 15. Turn off the pump. 16. Remove the yellow PEEK backpressure coil from the TO INJ VALVE IN - P/ELUENT OUT line and the mixer inlet. 17. Disconnect the mixer outlet from the TO SRS/AES REGEN OUT line and remove the 10-32 to 1/4-28 coupler. 18. Reconnect the TO SRS/AES REGEN OUT line to the suppressor REGEN OUT port.
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B-75
ICS-2000 Ion Chromatography System
Completing the Eluent Generator Setup for Carbonate/Bicarbonate Eluent
Figure B-74 illustrates the liquid flow path through the ICS-2000 after all setup steps are complete and the eluent generator is ready for operation. To the pump Degas In EGC Vent
EGC II K2CO3 Deionized Water
Inlet
Outlet Eluent Out Regen Out
EGC Degas
Eluent In
EPM Backpressure Coil
Regen In
Regen In Eluent In
Column Heater
Heat Exchanger
Cell Out
Suppressor
Regen Out
Degas Out Conductivity Cell Cell In
Eluent Out
Degas In
Press. Xducer.
C
W L
Separator
L
P
EGC CO3 Mixer
Pulse Damper Valve
S
Sample in
To waste
Pump Head
Guard
To waste Pump Head
To Gas Separator Assembly
Eluent Valve
Figure B-74. ICS-2000 Flow Schematic: Carbonate/Bicarbonate Eluent Generation
B-76
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Setting Up the Eluent Generator
1. Connect the TO INJ VALVE IN - P/ELUENT OUT line to the coupler attached to the mixer inlet line. Route this line along the back of the drip tray to prevent it from being pinched when the ICS-2000 door is opened and closed 2. Route the mixer outlet line to the back of the component panel (see Figure B-75). 3. Connect the mixer outlet line to port P (2) on the injection valve.
Figure B-75. Mixer Outlet Routed to the Back of the Component Panel NOTE Backpressure tubing may be required between the injection valve and the EGC CO3 Mixer outlet. The EluGen cartridge requires 14 to 16 MPa (2000 to 2300 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. See Section B.16.1 for details.
Go on to Section B.15.
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B-77
ICS-2000 Ion Chromatography System
B.14.3 Eluent Generator Setup for Carbonate Eluent Follow the instructions in this section if you are installing a K2CO3 cartridge and an EGC CO3 Mixer (for generating carbonate eluent).
• •
If you are installing a KOH, LiOH, MSA, or NaOH EluGen cartridge and a CR-TC, go to Section B.14.1. If you are installing a K2CO3 cartridge, an EPM, and an EGC CO3 Mixer (for generating carbonate/bicarbonate eluent), go to Section B.14.2.
Overview
The eluent generator setup procedure for carbonate eluent consists of the following main steps:
•
Installing the EluGen cartridge and preparing for conditioning.
•
Conditioning the EluGen cartridge.
•
Installing the EGC CO3 Mixer.
• •
B-78
Filling the EGC CO3 Mixer with the eluent concentration required for the application. Completing the eluent generator setup.
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Setting Up the Eluent Generator
Items Required to Complete the Setup Procedure
In addition to the EluGen cartridge and the EGC CO3 Mixer, you will need the following items to complete the eluent generator setup. Except as noted, all items are supplied in the ICS-2000 Ship Kit (P/N 064375).
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Item
P/N
Use To
Yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil
053765
Provide backpressure during setup procedures
EluGen Cartridge Vent Line Tubing Kit (supplied with the cartridge)
063092
Vent the cartridge during operation
EGC CO3 Mixer mounting clips
063642
Install the mixer
Phillips head screwdriver (not supplied)
n/a
Install the EGC CO3 Mixer mounting clips
35 cm (14 in) of black 0.25-mm (0.010-in) ID PEEK tubing
064346
Connect the EGC degas eluent outlet and the EGC CO3 Mixer inlet
60 cm (24 in) of black 0.25-mm (0.010-in) ID PEEK tubing
064343
Connect the EGC CO3 Mixer outlet to port P (2) on the injection valve
Temporary waste container (beaker, bottle, etc.) (not supplied)
n/a
Collect waste during setup procedures
10-32 fittings 10-32 ferrules
043275 043276
Complete the plumbing connections
1/8-in fittings 1/8-in ferrules
052267 048949
Complete the plumbing connections
10-32 to 10-32 couplers
042627
Complete the plumbing connections
B-79
ICS-2000 Ion Chromatography System
Figure B-76 illustrates the liquid flow path through the eluent generator components after all setup steps are complete and the eluent generator is ready for operation.
EGC VENT
EGC II K2CO3
Send to waste Outlet
Inlet EGC IN
TO DEGAS ELUENT IN TO DEGAS ELUENT OUT
EGC OUT
EGC DEGAS
TO EGC CO3 MIXER OUT
EGC CO3 Mixer
TO INJ VALVE IN - P ELUENT OUT TO PUMP/ DAMPER
Pre-plumbed to Pump Pulse Damper
Backpressure Coil* WASTE, GAS SEPARATOR
TO INJ VALVE PORT P
TO EGC CO3 MIXER IN
Connect to Inject Valve Port P (2) *Add backpressure coils, if needed, to create a system backpressure of between 14 and 16 MPa (2000 and 2300 psi).
TO SRS/AES REGEN OUT
Connect to Connect to Suppressor Gas Separator Regen Out Assembly
Figure B-76. Eluent Generator Flow Schematic with an EGC CO3 Mixer: Use for Generating Carbonate Eluent
B-80
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Setting Up the Eluent Generator
Installing the EluGen Cartridge and Preparing for Conditioning
Follow the steps in this section to install the EluGen cartridge and prepare it for conditioning before initial use. Figure B-77 illustrates the liquid flow path during the conditioning procedure.
EGC VENT
EGC II K2CO3
Send to waste Outlet
Inlet EGC IN
TO DEGAS ELUENT IN TO DEGAS ELUENT OUT
TO INJ VALVE IN - P/ ELUENT OUT
Backpressure Coil
EGC OUT
EGC DEGAS
14 MPa (2000 psi) at 1.0 mL/min
TO SRS/AES REGEN OUT
TO PUMP/ DAMPER
Pre-plumbed to Pump Pulse Damper
WASTE, GAS SEPARATOR
To waste
Connect to Suppressor Regen Out
Connect to Gas Separator Assembly
Figure B-77. EluGen Cartridge Plumbing for Conditioning with Carbonate Eluent
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B-81
ICS-2000 Ion Chromatography System
1. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the cartridge INLET and OUTLET fittings (see Figure B-54).
OUTLET
INLET
Figure B-78. EluGen Cartridge Fitting Plugs
2. Set the EluGen cartridge in the service area on top of the ICS-2000 and orient it with the cable toward the EGC holder (see Figure B-79).
EGC Cable
Figure B-79. EluGen Cartridge in Service Area
B-82
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Setting Up the Eluent Generator
3.
Pull the coiled black EGC IN and EGC OUT lines out from inside the EGC holder. Disconnect the EGC IN line from the coupler that connects it to the EGC OUT line.
4.
Connect the EGC IN line to the EluGen cartridge INLET port (see Figure B-80).
5.
Remove the coupler and connect the EGC OUT line to the EluGen cartridge OUTLET port.
Figure B-80. EluGen Cartridge Port Connections
6. Turn the EluGen cartridge over (with the fittings facing down). Shake the EluGen cartridge vigorously, and tap it with the palm of your hand 10 to 15 times. Check that all bubbles trapped in the eluent generation chamber are dislodged. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear protective eyewear and gloves when handling the cartridge. La cartouche d'EluGen contient un de ce qui suit: une base corrosive (KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution concentrée de K2CO3. Porter des lunettes et des gants protectives en manipulant la cartouche. Die EluGen-Kassette enthält eine korrodierende Base (KOH, LiOH oder NaOH), eine korrodierende Säure (MSA) oder eine konzentrierte K2CO3-Lösung. Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe.
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B-83
ICS-2000 Ion Chromatography System
7.
Slide the EluGen cartridge down into the holder until it stops (see Figure B-81). Make sure the cable remains out of the holder. NOTE To avoid crimping the lines, do not twist the cartridge when you slide it into the holder. The lines are designed to coil inside the holder.
Figure B-81. EluGen Cartridge Installed in the Holder
8.
Remove the plug from the EGC-1 connector on top of the ICS-2000.
9.
Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure B-82. Push it onto the EGC-1 connector on the ICS2000. Twist the ring on the cable connector fingertight to secure it.
Figure B-82. Connecting the EluGen Cartridge Cable
B-84
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Setting Up the Eluent Generator
10. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from port P (2) on the injection valve. 11. Use a 10-32 to 10-32 coupler (P/N 042627) to connect the TO INJ VALVE IN - P/ELUENT OUT line to one end of the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) (see Figure B-83). 12. Direct the free end of the backpressure coil to a temporary waste container.
EGC Cable
TO INJ VALVE IN - P/ ELUENT OUT
Backpressure Coil
Temporary Waste Container
Figure B-83. Plumbing Connections for Conditioning the EluGen Cartridge with Carbonate Eluent
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B-85
ICS-2000 Ion Chromatography System
Installing the EluGen Cartridge Vent Line
1. Locate the EluGen Cartridge Vent Line Tubing Kit (P/N 063092) supplied with the EluGen cartridge. 2. Slide the label onto one end of the tubing and then push the barbed luer lock onto the tubing. 3. Unscrew and remove the plug from the vent opening on the side of the EluGen cartridge (see Figure B-84).
Vent Plug (remove)
Figure B-84. EluGen Cartridge Vent Plug
4. Screw the luer adapter onto the vent opening. Remove the cap on the luer adapter by twisting. Save the cap.
Luer Adapter
Luer Lock
EGC Vent Line
5. Twist the luer lock and EluGen cartridge vent line into the luer adapter (see Figure B-85). Figure B-85. Installing the EluGen Cartridge Vent Line NOTE To prevent leaks from the EluGen cartridge, always replace the luer adapter cap before moving the EluGen cartridge.
6. Direct the EluGen cartridge vent line to the rear of the ICS-2000 and snap it onto one of the tubing clips on the rear panel.
B-86
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Setting Up the Eluent Generator
7. Direct the vent line to the waste container and insert it down into the gas separator waste tube about 10 to 15 cm (4 to 6 in). Recording the EluGen Cartridge Serial Number in Chromeleon
The serial number is printed on the EluGen cartridge label. 1. Open the Chromeleon Server Configuration program (select Start>Programs (or All Programs)>Chromeleon>Server Configuration). 2. Double-click the ICS-2000 system icon. The properties dialog box for the ICS-2000 appears. 3. Click the Eluent Generator tab (see Figure B-86). 4. Select the EGC-1 check box. 5. Enter the EluGen cartridge serial number and click OK.
Figure B-86. Eluent Generator Configuration Properties Example
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B-87
ICS-2000 Ion Chromatography System
Conditioning the EluGen Cartridge
After completing the installation steps described in the previous sections, condition the EluGen cartridge for 30 minutes before initial use. 1. Make sure the eluent reservoir is filled with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor is off. To avoid damaging the suppressor, always turn off the suppressor before conditioning the EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor.
3. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 4. On the ICS-2000 touch screen HOME page, set the pump flow rate to 1.00 mL/min. 5. Turn on the pump. 6. On the touch screen HOME page, touch the EGC button to open the ELUENT GENERATOR page. Verify that the cartridge type is Carb. If the cartridge type is wrong, verify that the cartridge serial number was entered correctly in the Chromeleon Server Configuration program (see “Recording the EluGen Cartridge Serial Number in Chromeleon” on page B-87). 7. Set the EGC-1 concentration to 9 mM. 8. Turn on the EGC-1 current. 9. Run the EluGen cartridge at these settings for 30 minutes. 10. Turn off the EGC-1 current. 11. Turn off the pump.
B-88
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Setting Up the Eluent Generator
Installing the EGC CO3 Mixer
Figure B-67 illustrates the EGC CO3 Mixer after installation.
TO EGC CO3 MIXER OUT (P/N 064343)
TO EGC CO3 MIXER IN (P/N 064346)
Figure B-87. ICS-2000 with an EGC CO3 Mixer Installed
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B-89
ICS-2000 Ion Chromatography System
1. Use a Phillips head screwdriver to remove the existing small diameter mounting clips from the inside of the ICS-2000 door. 2. Install the larger diameter mounting clips (P/N 063642) (see Figure B-88). Mixer Mounting Clips
Figure B-88. Location of Mounting Clips for the EGC CO3 Mixer
3. Orient the mixer with the outlet pointing upward and push it onto the clips (see Figure B-89). The mixer outlet must point upward to ensure thorough mixing of the eluent.
Mixer Outlet
4. Locate the 35 cm (14 in) length of black PEEK tubing (white labels) (P/N 064346). Connect the end labeled TO EGC CO3 MIXER IN to the mixer inlet. 5. Locate the 60 cm (24 in) length of black PEEK tubing (white labels) (P/N 064343). Connect the end labeled TO EGC CO3 MIXER OUT to the mixer outlet.
Mixer Inlet
Figure B-89. EGC CO3 Mixer Installed on the ICS-2000 Door
B-90
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Setting Up the Eluent Generator
Filling the EGC CO3 Mixer with the Carbonate Eluent
Before initial use, follow the steps in this section to fill the EGC CO3 Mixer with the carbonate eluent required for the application to be run. Figure B-90 illustrates the liquid flow path through the eluent generator components during initial filling of the EGC CO3 Mixer with carbonate eluent.
EGC VENT
EGC II K2CO3
Send to waste Outlet
Inlet EGC IN
TO DEGAS ELUENT IN
EGC OUT
EGC DEGAS
TO DEGAS ELUENT OUT
TO EGC CO3 MIXER OUT
TO INJ VALVE IN - P/ ELUENT OUT
EGC CO 3 Mixer TO SRS/AES REGEN OUT
TO PUMP/ DAMPER
Pre-plumbed to Pump Pulse Damper
WASTE, GAS SEPARATOR
Back14 MPa (2000 psi) pressure at 1.0 mL/min To waste Coil TO EGC CO3 MIXER IN
Connect to Suppressor Regen Out
Connect to Gas Separator Assembly
Figure B-90. Plumbing for Filling the EGC CO3 Mixer with Carbonate Eluent
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B-91
ICS-2000 Ion Chromatography System
1. Connect a 10-32 to 10-32 coupler to the mixer inlet and connect the outlet of the yellow PEEK backpressure coil to the coupler. 2. Direct the mixer outlet to the temporary waste container. 3. Verify that the suppressor is off. To avoid damaging the suppressor and CR-TC, always turn off the suppressor before conditioning the EluGen cartridge. The pump flow is on during conditioning, however, no flow reaches the suppressor.
4. Verify that the Automatically turn on with pump option is not selected on the ICS-2000 touch screen SUPPRESSOR page (see Section C.9). Disabling this option lets you turn on the pump, without automatically turning on the suppressor. 5. Set the pump flow rate to the rate required for the application. 6. Turn on the pump. 7. Verify that the system backpressure is between 14 and 16 MPa (2000 and 2300 psi). If necessary, adjust the pressure by adding or removing backpressure tubing. 8. Set the EGC-1 concentration to the value required for your application. 9. Turn on the EGC-1 current. 10. Run at these settings until a consistent flow of eluent is exiting the mixer outlet. At a flow rate of 1 mL/min it will take about 16 minutes to fill a 4-mm mixer and about 5 minutes to fill a 2-mm mixer. NOTE The void volume of the 4-mm mixer is about 16 mL. The void volume of the 2-mm mixer is about 5 mL.
11. Turn off the EGC-1 current. 12. Turn off the pump. 13. Remove the yellow PEEK backpressure coil from the TO INJ VALVE IN - P/ELUENT OUT line and the mixer inlet. 14. Retain the coupler on the mixer inlet.
B-92
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Setting Up the Eluent Generator
Completing the Eluent Generator Setup for Carbonate Eluent
Figure B-91 illustrates the liquid flow path through the ICS-2000 after all setup steps are complete and the eluent generator is ready for operation.
To the pump Degas In EGC Vent
EGC II K2CO3 Deionized Water
Inlet
Outlet
EGC Degas
Backpressure Coil
Degas In
Eluent Out
Heat Exchanger
Suppressor
Regen In
Cell Out
Regen Out
Eluent In
Degas Out Conductivity Cell Cell In
Column Heater
Press. Xducer.
C L
P
To waste
Eluent Valve
Pump Head
To waste Guard
Pump Head
Sample in
EGC CO3 Mixer
L
W
Separator
Pulse Damper Valve
S
To Gas Separator Assembly
Figure B-91. ICS-2000 Flow Schematic: Carbonate Eluent Generation
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B-93
ICS-2000 Ion Chromatography System
1. Connect the TO INJ VALVE IN - P/ELUENT OUT line to the coupler attached to the mixer inlet line. Route this line along the back of the drip tray to prevent it from being pinched when the ICS-2000 door is opened and closed. 2. Route the mixer outlet line to the back of the component panel (see Figure B-92). 3. Connect the mixer outlet line to port P (2) on the injection valve.
Figure B-92. Mixer Outlet Routed to the Back of the Component Panel NOTE Backpressure tubing may be required between the injection valve and the EGC CO3 Mixer outlet. The EluGen cartridge requires 14 to 16 MPa (2000 to 2300 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. See Section B.16.1 for details.
Go on to Section B.15.
B-94
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Setting Up a Chromeleon Application
B.15 Setting Up a Chromeleon Application Chromeleon provides application templates that let you quickly get started running. To use the application templates, you need to know the type of column and suppressor you will be using. This section shows how to create a sequence (a list of samples to be processed) and how to use an application template. 1. Identify the type of column and suppressor installed in the ICS-2000. 2. Start Chromeleon (select Start>Programs>Chromeleon>Chromeleon). The Chromeleon main window and Browser appear (see Figure B-93).
Figure B-93. Chromeleon Main Window and Browser
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B-95
ICS-2000 Ion Chromatography System
3. In the Browser, select File>New and select Sequence (using Wizard) (see Figure B-94).
Figure B-94. Creating a New Sequence
The Sequence Wizard Welcome page appears (see Figure ).
Figure B-95. Sequence Wizard Welcome Page
B-96
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Setting Up a Chromeleon Application
NOTE For details about a Sequence Wizard step, click the Help button on the Sequence Wizard page.
4. Click Next>. The Sequence Wizard Timebase page appears (see Figure B-96).
Figure B-96. Example: Sequence Wizard Step 1
5. Select the ICS-2000 timebase and click Next>.
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B-97
ICS-2000 Ion Chromatography System
The Unknown Samples page appears (see Figure B-97).
Figure B-97. Example: Sequence Wizard Step 2
6. Select Use Template from the drop-down list. 7. In the Template for Sample Name field, type Sample, click the right arrow, and select Sample Number #n. 8. In the Number of Vials field, type 1. 9. Use default settings for the remaining parameters on the page. NOTE You can edit the sequence later, to add more samples and select the injection parameters appropriate for your application.
B-98
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Setting Up a Chromeleon Application
10. Click Apply>>. Figure B-98 shows Sequence Wizard Step 2 after a sample is defined.
Figure B-98. Example: Sequence Wizard Step 2 with Sample Defined
11. Click Next>.
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B-99
ICS-2000 Ion Chromatography System
The Standard Samples page appears (see Figure B-99).
Figure B-99. Example Sequence Wizard Step 3
12. Click Next> to omit this step and define standard injections later. Or, define one or more standard injections, and then click Next>. The Methods & Reporting page appears.
B-100
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Setting Up a Chromeleon Application
13. Select the Use Application Template check box. 14. From the drop-down lists, select the type of suppressor to be installed and then select the column. In the example in Figure B-100, the 4-mm ASRS suppressor and AS17 column are selected.
Figure B-100. Example: Sequence Wizard Step 4
15. To select a report template, click the Browse button, go to the Dionex Templates/Reports folder, and select a template (for example, default). 16. Click Next>. The Saving the Sequence page appears.
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B-101
ICS-2000 Ion Chromatography System
17. Enter a name for the sequence and a location (see the example in Figure B-101).
Figure B-101. Example: Sequence Wizard Step 5
18. Click Finish> and then click Done on the last page of the Sequence Wizard.
B-102
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Setting Up a Chromeleon Application
The Browser appears, displaying the sequence you created (see Figure B-102). Notice the three files in the top pane of the Browser window.
Figure B-102. Example Browser with Open Sequence
• • •
The .pgm file (program) contains commands and parameters for controlling the ICS-2000, controlling the autosampler (if used), and acquiring sample data. The .qnt file (quantification method) contains peak identification and area determination parameters. The .pan file (Control panel) lets you control and/or monitor the ICS2000 and other modules that are connected to the timebase. NOTE The sequence that you create here is intended as a starting point only. You can add additional samples to the sequence, change injection parameters, and edit the .pgm and .qnt files. Refer to the Chromeleon online Help for details. NOTE After completing the installation, see Section 3.11 for how to process the samples and standards in the sequence.
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B-103
ICS-2000 Ion Chromatography System
19. Double-click the .pan file to open the Control panel for your system (see the example in Figure B-103).
Figure B-103. ICS-2000 System Control Panel Example NOTE If the Connected check box is not selected, click the box to connect the ICS-2000 to the Control panel.
B.15.1 Verifying Chromeleon Communication Verify that Chromeleon is communicating with the ICS-2000 by clicking the Inject and then the Load button on the Control panel. If communication is occurring, you will hear the valve actuate as it changes position. Go on to Section B.12.
B-104
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Equilibrating the System
B.16 Equilibrating the System 1. After priming the pump, turn on the pump and set the flow to the operating rate. 2. Flush the system for about 5 minutes to equilibrate. 3. Monitor the system pressure reading from the Chromeleon Control panel. The EluGen cartridge requires at least 14 MPa (2000 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. A system backpressure of 16 MPa (2300 psi) is ideal. If the pressure is too low, install a backpressure coil (see Section B.16.1). The recommended maximum operating pressure for the eluent generator is 21 MPA (3000 psi). Excessive backpressure may rupture the tubing in the EGC degas tubing assembly.
4. Check that liquid is flowing out of the suppressor REGEN OUT waste line and that the pressure is stable. 5. Monitor the baseline conductivity. In general, it should be Chromeleon > Chromeleon.
F.8
How do I delete data? In the Chromeleon Browser, highlight the sequence you want to delete and then select File >Delete.
F.9
How do I back up data? In Chromeleon, select File >Export/Backup. Back up the data and indicate the backup source.
F.10 How do I shut off the system? In Chromeleon, click the System Shutdown button on the Control panel (see Figure 2-11). On the ICS-2000, turn off the power switch on the rear panel (see Figure 2-9).
F.11 How do I store columns? Columns should be stored in eluent. See the column manual for complete instructions. The column manual is included on the Dionex Reference Library CD-ROM (P/N 053891).
F-2
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F • FAQ
F.12 How do I know when a column is dirty? See the troubleshooting section of the column manual.
F.13 How do I clean a column? See the troubleshooting section of the column manual.
F.14 Why is the conductivity high? Possible reasons for high conductivity include:
•
The suppressor needs regeneration. See the suppressor manual for troubleshooting information. The suppressor manual is included on the Dionex Reference Library CD-ROM (P/N 053891).
•
The cell is out of calibration. See Section 5.1.3 for calibration instructions.
•
See Section 4.12 for additional troubleshooting information.
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F-3
ICS-2000 Ion Chromatography System
F-4
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G • Glossary Analytical Column Synonymous with Separator Column. Band Spreading The broadening of the sample band as it travels through the column. Band spreading can also occur in the injection valve, detector cell, and interconnecting tubing. Calibration Curve A graph showing detector response in peak height or area versus analyte concentration. Capacity Factor (k´) The number of column volumes of eluent, pumped through the column, required to elute an analyte. Capacity factor is a dimensionless measure of retention which is independent of column length or eluent flow rate. It is calculated as follows:
tr – to k′ = ------------to
Where: tr = retention time to = retention time of unretained solute (column void volume)
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G-1
ICS-2000 Ion Chromatography System
Cell Constant (k) A factor determined experimentally by measuring the conductance (G) of a standard solution of known equivalent conductivity (k).
k = κ⁄G The value of k depends upon the surface area of, and distance between, the electrode faces in the conductivity detector cell.
k = l⁄A Where: l = length A = area of one electrode (the other electrode is equal to the first) Channeling The preferential flow of liquid along more open, less resistant paths through the column packing. This causes Band Spreading. Column Efficiency (N) A measure of the narrowness of analyte bands as they elute from the column. High efficiency is desirable because resolution between closely spaced bands improves with greater efficiency. For a symmetrical (Gaussian) peak, column efficiency can be determined by the following: N = 5.54(t1/W1/2)2 Where: t1 = the peak retention time (in seconds) W1/2 = the peak width at 1/2 height (in seconds) Column efficiency is proportional to column length: for a given resin and column diameter, increasing the column length increases the column efficiency. Synonymous with Theoretical Plates. Column Selectivity (a) Describes the relative separation of the band maxima between two adjacent peaks. Selectivity can be determined by the following: a = (t2 - t0)/(t1 -t0) Where: t1 and t2 = retention time of components 1 and 2, respectively t0 = retention time of unretained components (void volume) Concentrator Column A short column used to retain and concentrate analytes from a measured volume
G-2
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G • Glossary
of relatively clean sample. This allows large volumes of sample to be injected, lowering concentration detection limits. Conductivity A measure of the ease with which electrical current flows through a liquid contained between two opposite charged electrodes. Conductivity is a characteristic of ions in solution. Units are siemens. Counterion Ions carrying a charge opposite that of the sample ions (e.g., Na+) may be the counterion of a Cl- analyte. These ions preserve electrical neutrality in solution. % Crosslink Divinylbenzene content in a polystyrene/divinylbenzene (PS-DVB) resin; this contributes to the mechanical strength of the resin and determines chromatographic properties. Equivalent Conductivity (λ) The contribution of an ionic species to the total conductivity of a solution as measured in a standard cell having electrodes 1 cm2 in area and exactly 1 cm apart. Guard Column A small column that prevents poisoning of the separator column by sorbing organic contaminants and removing particulates. It is filled with the same packing as the separator column. Synonymous with Pre-Column. HETP (H) Height Equivalent to a Theoretical Plate. A measure of column efficiency which allows comparison between columns of different lengths. HETP = H = L/N Where: L = the column length (in mm) N = the number of theoretical plates Ion-Exchange Capacity The number of active ion exchange sites in a given weight or volume of resin; this is usually expressed in meq/g or meq/mL. Ion-Exchange Resin An insoluble polymer matrix containing fixed-charge exchange sites (anionic or cationic). IC resins are formed into small spherical particles (beads).
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G-3
ICS-2000 Ion Chromatography System
Packing The material that fills a chromatographic column; usually a resin or silica-based material. Pellicular Resin A resin with a solid, nonporous core coated with a thin layer of more porous material. The exchange sites of pellicular ion exchange resins are located only on the surface layer of the bead. These resins have a low ion-exchange capacity. Pre-Column Synonymous with Guard Column. Regenerant A dilute acid or base that converts ion exchange sites in a MicroMembrane Suppressor back to the form that suppresses the eluent conductivity. Resin See Ion-Exchange Resin. Resolution (R) A measure of the separation between two sample components. This is expressed as the ratio of the distance between the two peak maxima to the mean value of the peak width at the baseline. R = 2(t2 - t1)/(W2 + W1) Where: t1 and t2 =the retention times of components 1 and 2, respectively W1 and W1 = the baseline width of peaks 1 and 2, respectively (measured in the same units as the retention time) R is proportional to the square root of efficiency (N). A value of R = 1.5 represents “baseline separation” of the two peaks. Retention Time The time from injection to peak maximum; the basis for identification of a species in chromatographic analysis. Separator Column The column used to perform a chromatographic separation; also called an analytical column.
G-4
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G • Glossary
Siemens (S) Unit measure of conductance; the reciprocal of the electrical resistance of a solution. Suppressor A device used to minimize eluent conductivity and convert sample species to a common form, thus increasing detection sensitivity. Temperature Coefficient The percent of change in the conductivity of a solution with a 1 oC change in temperature. Every solution has a characteristic temperature coefficient which is determined experimentally. Theoretical Plates (N) See Column Efficiency. Void Volume (V0) The volume occupied by the eluent in a packed column. This volume includes the volume between the injection valve and the column, as well as between the column and the detector cell. Unretained components are eluted in the void volume.
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G-5
ICS-2000 Ion Chromatography System
G-6
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Index
Symbols % Offset (analog out), C-26
A Adjusting the contrast, 2-2, C-1 Air particulate samples, 3-13 Air regulator, B-114 – B-115 Alarm conditions, 4-3 – 4-11 See also Error messages Ambient temperature, 4-22 Analog output, C-24, C-26, D-2 % Offset, C-26 Configuring, C-26, D-10 Connections, D-10 Connector, 2-10 Full scale, C-26 Range, C-26 Analog-to-digital controller, D-10 Anion separations, 2-35, 3-12 AS/AS50 (USB) Autosampler Connections for stand-alone operation, D-7 Enabling injection valve control, D-9 Installation, B-107 Method for stand-alone operation, D-11 Sample injection, 3-16 Schedule for stand-alone operation, D-11 Time Function Out screen, D-9 Yearly maintenance, 3-22 AS40 Automated Sampler Installation, B-111 Sample injection, 3-16 Yearly maintenance, 3-22 Atlas Electrolytic Suppressor, 2-9 See also Suppressor
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Audit Trail, 2-16 Error messages, 4-1 Icons, 4-1 Automated control, 2-12 Autosampler Loading samples with, 3-16 See also AS/AS50 (USB) Autosampler See also AS40 Automated Sampler Autozero, 2-19, 3-12, 3-19, C-9
B Background conductivity High, 4-21 Offsetting, 2-19, 3-12, C-9, C-11 Backlight Time-out, C-28 Backpressure, 2-34 Restriction in plumbing, 5-10 Troubleshooting, 4-18 Backpressure coil, 2-38 Backpressure, low How to increase, 2-38 Bar, C-17 Baseline Drift, 4-22 Equilibration, B-105 Noise, 4-22, C-25 Stability, 2-43 Zeroing, 2-19, C-9 Batch processing, 3-2 Starting, 3-20 See also Sample processing Blockages Liquid lines, 4-9, 5-10 Browser, 2-12, 3-5, B-118 Busy page, C-28
Index-1
ICS-2000 Ion Chromatography System
C Cables AS40 Relay Control, B-111 Power cord, 5-37 USB, B-10 Calibration, 5-1 Conductivity cell, 5-5 Flow rate, 5-7 Vacuum degas assembly, 5-9 Carbonate eluent, 2-23, 2-35, 2-39 Carbonate/bicarbonate eluent, 2-23, 2-35, 2-39 Cation separations, 2-35, 3-12 Cell See Conductivity cell Cell calibration, 5-5 Cell drive, A-3 Cell heater, C-9 Check valves Cleaning procedure, 5-16 – 5-17 Replacement procedure, 5-16 – 5-17 Chromatogram, 1-3 Zeroing the baseline, 2-19, C-9 Chromeleon, 2-12 Adding devices to a timebase, B-20 Alarm conditions, 4-3 Audit Trail, 4-1 Audit Trail error messages, 4-1 Browser, 2-12, 3-5 Control panel, 2-12, 3-18 Creating a sequence, 3-20 Degas options, 4-23 Direct control, 2-12 Error messages, 4-3 Installation, B-5, B-15 Interface, 2-12 License installation, B-5 – B-6 Menu, 2-12, 3-18 Programs, 2-12, 2-15, 3-16 – 3-18 Starting, 3-4, B-95 System properties dialog box, B-19 Timebase, 3-5 Toolbars, 2-12, 3-18
Index-2
Using the touch screen with Chromeleon, C-4 Verifying communication, B-104 Wellness panel, 5-1 Chromeleon Server Starting, 3-4, B-13 Chromeleon Server Configuration program Timebase, B-18 Column heater, 2-8, 2-42 Chromeleon control, 2-18 Home page control, C-8 Replacement procedure, 5-29 Specifications, A-4 Column heater alarms Column heater exceeds safe temperature, 4-3 Column heater open circuit, 4-3 Column heater short circuit, 4-3 Columns, 2-8 Cleaning, F-3 Contaminated, 4-20 Damage from IPA, 5-37 Installing, B-23 Storing, F-2 Commands Chromeleon, 2-12, 3-19, B-103 Component panel, 2-7 Computer Connections, B-10 Operating system requirements, B-5 Unpacking, B-4 Concentration, C-20 Upper limits, 4-6, C-20 See also EGC Conductivity, C-9 Causes of high conductivity, F-3 Changing the display, C-28 Offset, C-9, C-28 Temperature effect, 2-43 Total, C-9, C-28
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Index Conductivity cell, 2-9, 2-43 Calibrating, 5-5 Calibration constant, 5-26 High cell output, 4-21 Leaking, 4-14 No response, 4-20 Replacement procedure, 5-25 Setting the temperature, C-9 Specifications, A-3 Volume, 2-43 Conductivity cell specifications Active volume, A-3 Cell body, A-3 Electrodes, A-3 Maximum pressure, A-3 Conductivity polarity, C-25 Contacting Dionex, 5-1 Contamination Column, 4-19 – 4-20 Eluents, 4-19 Sample, 4-20 Standard, 4-19 Continuously Regenerated Trap Column See CR-TC Control panel (Chromeleon), 2-12 – 2-13, 3-18 System panel, 2-13 – 2-17, 2-19 Wellness panel, 2-13 CR-TC, 2-38 Connector, 2-6 Controlling automatically, C-22 Controlling manually, C-22 Home page control, C-8 Replacement, 5-60 CR-TC alarms CR-TC over current error, 4-4 CR-TC stopped for zero flow rate, 4-4 Current, C-23
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D Daily maintenance, 3-21 Data Backing up, F-2 Deleting, F-2 Filtering, C-25 Saving, 3-18 – 3-19 Data acquisition, 3-19 Data analysis description, 1-3 Data rise time, B-113, C-24 – C-25 Decibel level, A-1 Degas tubing assembly See Vacuum degas assembly Degas calibration failed alarm, 4-4 Degas tubing assembly, eluent generator, 2-35, 2-37 Degassing eluents, 2-30 Delay volume, A-2 Detection description, 1-3 Detector controls on Control panel, 2-19 Detector controls on Home page, C-9 See also Conductivity cell Detector page, C-24 Setting analog out options, C-26 Setting the data rise time, C-25 Detector specifications Cell drive, A-3 Linearity, A-3 Range, A-3 Temperature compensation, A-3 Diagnostic pages, C-30 Diagnostics, 5-1 Dimensions, A-1 Dionex Contacting, 5-1 Direct control, 2-12 Dongle, B-6 Drip tray, 2-8 DS6 Heated Conductivity Cell See Conductivity cell Duty cycle, 2-31, C-18
Index-3
ICS-2000 Ion Chromatography System
E EGC, 2-6 Backpressure requirement, 2-38, 2-41 Concentration ranges, 2-36 Concentration upper limits, 4-6, C-20 EGC-1 connector, 2-6, 5-44, 5-52, B-45, B-61, B-84 EGC-2 connector, 2-6 Eluent types, 2-35 Entering the serial number, C-19 Expiration date, C-21 Home page controls, C-8 Installation, B-35 Life remaining percentage, 2-21, C-21 Service area, 2-7 Vent line installation, B-37, B-53, B-61, B-79, B-86 See also Eluent generator EGC alarms EGC board not present, 4-5 EGC-1 calibration error, 4-5 EGC-1 disconnected error, 4-5 EGC-1 invalid concentration vs flow rate error, 4-6 EGC-1 invalid flow rate error, 4-6 EGC-1 over-current, 4-6 EGC-1 over-voltage, 4-7 EGC CO3 Mixer Description, 2-35, 2-39 Flow schematics, 2-23 Replacement procedure, 5-69 EGC Resistive Load, 5-4 EGC Verification, 5-4 EGC-1 connector, 2-6, 5-44, 5-52, B-45, B-61, B-84 EGC-2 connector, 2-6 Elapsed time, C-9, C-11 Electrical specifications Fuses, A-1 Main power, A-1 Electrolysis gases Purging from eluent, 2-38, 2-41
Index-4
Electrolytic pH modifer See EPM Electrolytic pH Modifier Eluent Aqueous, 3-22, 4-16 Concentration, C-20 Degassing, 2-30 Delivery process, 1-2 Filtering, 3-6 See also Eluent generator Eluent bottle See Eluent reservoir Eluent concentration, 2-36 Eluent generator, 2-6, 2-35 Backpressure, 2-41 Chromeleon control, 2-20 – 2-21 Controlling automatically, C-21 Controlling manually, C-21 Degas tubing assembly, 2-35, 2-37 EGC holder, 2-37, B-40, B-56 EGC replacement procedure, 5-38 EGC types, 2-35 Electrolysis gases, 2-38, 2-41 Eluent concentration ranges, 2-36 Installation, B-35 Setting the concentration, C-20 Specifications, A-4 See also EGC Eluent Generator page, C-19 Eluent level, 3-7, B-30, C-7 Eluent reservoir Connecting, 3-9, B-29 Filling, 3-7 Gas connection, B-114 Monitoring liquid level in, 3-7, B-30, C-7 Pressurization, B-115 Eluent valve, 2-8, B-33, C-18 Chromeleon control, 2-17 Replacing, 5-33 EluGen cartridge See EGC End-line filter See Filter, end-line
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Index Environmental specifications Humidity, A-1 Operating pressure, A-1 Operating temperature, A-1 EPM Electrolytic pH Modifier, 2-6, 2-38 – 2-39 Normalized Life, 2-21 Replacement procedure, 5-64 Equilibration time, 3-12 Error messages, 4-3 – 4-11 Audit Trail description, 4-1 Column heater exceeds safe temperature, 4-3 Column heater open circuit, 4-3 Column heater short circuit, 4-3 CR-TC over current error, 4-4 CR-TC stopped for zero flow rate, 4-4 Degas calibration failed, 4-4 EGC board not present, 4-5 EGC-1 calibration error, 4-5 EGC-1 disconnected error, 4-5 EGC-1 invalid concentration vs flow rate error, 4-6 EGC-1 invalid flow rate error, 4-6 EGC-1 over-current, 4-6 EGC-1 over-voltage, 4-7 Hardware not present, 4-7 Leak sensor wet, 4-7 Load/inject valve error, 4-8 Option not installed, 4-8 Pressure slope calibration error, 4-8 Pump motor lost control, 4-9 Pump over pressure, 4-9 Pump pressure hardware error, 4-9 Pump under pressure, 4-10 Suppressor not connected, 4-11 Suppressor over current, 4-10 Suppressor over power, 4-10 – 4-11 Suppressor stopped for zero flow rate, 4-11
F Facility requirements, B-1
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Filter, end-line Bacterial contamination, 3-22, 4-16 Dirty or clogged, 3-22, 4-15 Installation, 3-6 Filtering data, C-25 Fittings Leaking, 4-12 Replacing, 5-14 Requirements, 5-14 Flow description Carbonate eluent generation, 2-29 Carbonate/bicarbonate eluent generation, 2-27 KOH, LiOH, MSA,NaOH eluent generation, 2-25 Flow rate, 2-8, A-2, C-6 Calibration, 5-7 Troubleshooting, 4-17 Flow schematics, 2-23 Carbonate eluent generation, 2-28, B-93 Carbonate/bicarbonate eluent generation, 2-26, B-76 KOH, LiOH, MSA, NaOH eluent generation, 2-24 FROM PC USB connections, B-10 Front panel, 2-1 Specifications, A-2 See also Touch screen Full-scale analog output, C-26 Fuses Replacement procedure, 5-37 Requirements, A-1
G Gas separator waste tube, 2-35, B-27 Installation, B-28 Gas source Connection, B-114 Installation, B-114 Pressure requirement, B-114 Ghosting, 4-19
Index-5
ICS-2000 Ion Chromatography System Guard column, 2-8, B-23 Installation, B-24
H Hardware not present error, 4-7 Heater, column, 2-42 See also Column heater High pressure alarm, 4-9 High pressure limit, A-2 Home page, 2-2, C-1, C-6, C-8 – C-10 Column Heater control, C-8 Detector controls, C-9 EGC controls, C-8 Injection valve controls, C-9 Pump controls, C-6 Humidity limits, A-1
I Information page, C-27 Injecting samples, 3-14 Via autosampler, 3-16 Via syringe, 3-15 Via vacuum syringe, 3-16 Injection port, 2-1 Injecting via syringe, 3-15 Injection valve, 2-8, 2-40 Chromeleon control, 2-18 Controlling with an AS50, D-9 Home page controls, C-9 Leaking, 4-13 Plumbing connections, 2-40 Rebuilding, 5-15 Specifications, A-3 Troubleshooting, 4-8 Input/Output page, C-29, D-9 Installation, B-1 – B-120 Adding devices to a timebase, B-20 Analog output connection, D-10 AS/AS50 (USB) Autosampler, B-107 AS40 autosampler, B-111
Index-6
Assigning devices to a timebase, B-18 Chromeleon, B-5, B-15 Columns, B-23 Computer, B-4 EGC vent line, B-37, B-53, B-61, B-79, B-86 Eluent generator, B-35 Eluent reservoir, B-29, B-115 Equilibrating the system, B-105 Gas separator waste tube, B-27 Gas source, B-114 Guard column, B-24 Key code, B-9 Operating system requirements, B-5 Operational status verification, B-106 PC connections, B-10 Plumbing, B-29 Power connection, B-12 Priming, B-31 – B-34 Separator column, B-24 Software license, B-5 – B-6 Stand-alone operation setup, D-7 – D-8 Starting the ICS, B-13 Suppressor, B-25 TTL and relay connections, D-1 – D-2 Unpacking, B-2 USB connections, B-10 – B-11 Waste lines, B-27 Installation troubleshooting, B-120 Installed options, C-27 Inverted edge TTL input control, D-5 Inverted peaks, C-25 Inverted pulse TTL input control, D-5 Ion chromatography Overview, 1-1 Ion exchange, 1-3 IonPac ATC-HC Trap Column, 2-38 IonPac CTC-1 Trap Column, 2-38 Isopropyl alcohol, 5-36 – 5-37
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Index
K
M
Key code (Chromeleon), B-6 KOH EGC, 2-35
Main power receptacle, 2-11 Maintenance, 3-21 Daily, 3-21 Ongoing, 3-21 Weekly, 3-22 Yearly, 3-22 Manual sample processing, 3-2 Methanesulfonic acid eluent, 2-35 MicroMembrane Suppressor, 2-9 See also Suppressor Module Setup page, C-28 Moduleware, 4-1, C-27 MPa, C-17 MSA EGC, 2-35
L LCD screen, 2-1 – 2-2, C-1 Specifications, A-2 See also Touch screen Leak sensor, 2-8 Leak sensor wet alarm, 4-7 Replacement, 5-35 Leaks Cell, 4-14 Fittings, 4-12 Injection valve, 4-13 Liquid, 4-12 Pressure transducer, 4-13 Pump check valve, 4-12 Pump head, 4-13 Pump head waste valve, 4-13 Pump piston seal, 4-13 Suppressor, 4-13 LED, A-2 License (Chromeleon), B-5 – B-6 License server (Chromeleon), B-6 Linearity requirements, A-3 LiOH EGC, 2-35 Liquid leaks, 4-12 See also Leaks Lithium hydroxide eluent, 2-35 Load/inject valve alarm, 4-8 Loading samples, 3-14 Local Mode, C-10 Locked Remote mode, C-4 Loop See Sample loop Low pressure limit, A-2
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N NaOH EGC, 2-35 Nitrite in samples, 3-13 Noise, baseline, C-25 Normal edge TTL input control, D-4 Normal pulse TTL input control, D-5
O Offset conductivity, C-28 Offset percentage (analog out), C-26 Offsetting background conductivity, 2-19, 3-12, C-9 Operating features, 2-1 Operating pressure, A-1 Operating ranges Cell heater, 2-9, C-9 Column heater, 2-8, C-8 Eluent concentration, 4-6, C-20 Flow rate, 2-8, C-6 Operating system requirements, B-5 Operating temperature, A-1
Index-7
ICS-2000 Ion Chromatography System Operation Equilibration time, 3-12 Overview, 3-1 Priming, 3-10, 5-36, B-34 Reservoir setup, 3-6 Sample preparation, 3-13 Sample processing, 3-2 Setting operating conditions, 3-11 Starting Chromeleon, 3-4 System power-up, 3-3 Operational status verification, 3-12 Option not installed error, 4-8 Options installed, C-27 Oven See Column heater Overview, 1-4
P Panels Chromeleon Control panel, 2-12, 3-18 Chromeleon Wellness panel, 5-1 Component panel, 2-7 Parameters Chromeleon operating commands, 2-12, 3-19, B-103 PC See Computer Peak ghosting, 4-19 Peak height Effect of rise time on, C-25 Reproducibility, 2-43 Troubleshooting, 4-20 Peak shape, C-25 Peak width, C-25 Peaks Effect of rise time on, C-25 Extraneous (ghosting), 4-19 Inverted, C-25 Reversed, C-25 – C-26 PEEK Conductivity cell body, 2-43
Index-8
pH modifer See EPM Electrolytic pH Modifier Physical specifications Decibel level, A-1 Dimensions, A-1 Weight, A-1 Piston seals Replacement procedure, 5-18 – 5-19 Pistons Replacement procedure, 5-22 Plot offset, C-11 Plot page, C-10 – C-11 Elapsed time, C-11 Plot offset, C-11 Range, C-11 Plotting detector output, 2-19, C-11 Plottting detector output, 2-16 Plumbing Columns and suppressor, B-29 Injection valve, 5-15 Replacing tubing and fittings, 5-14 Troubleshooting, 5-10 Plumbing diagrams, 2-23 Polarity Selecting the conductivity polarity, C-25 Potassium carbonate eluent, 2-39 Potassium hydroxide eluent, 2-35 Power Turning on, 3-3, B-13 Power cord, 5-37, B-12 Power receptacle, 2-11, B-12 Power requirements, A-1 Power-up conditions, 3-3 Pressure Home page display, C-6 Limit, 4-10, C-6, C-16 Pump operating specifications, A-2 System, 4-10, C-16 Unit (selecting), C-16 Pressure ripple, A-2 Pressure slope calibration error, 4-8 Pressure transducer, 2-8, 2-34 Leaking, 4-13 System backpressure, 2-34 Doc. 031857-03 4/06
Index Pressurizing Eluent reservoir, B-115 Prime button, C-7 Priming, 3-10, 5-36, B-31 – B-34 Pump is out of prime, 4-15 With a syringe, B-32 With isopropyl alcohol, 5-36 With the Prime button, B-34 Priming valve Opening, 2-33 O-ring replacement procedure, 5-23 Printing, F-1 Problems See Troubleshooting Processing samples, 3-2, 3-18 – 3-19 Automatically (batch), 3-2, 3-19 Manually, 3-2, 3-18 Product warranty, 5-1 Programs (Chromeleon), 2-12, 2-15 AS/AS50 (USB) example, 3-17 AS40 example, 3-18 Controlling an autosampler, 3-16 Run time, 2-15 PSI, C-17 Pulse damper, 2-25, 2-27, 2-29, 2-34 Pump, 2-32 Chromeleon control, 2-17 Flow rate, 2-8, C-6 Home page controls, C-6 Leaks, 4-13 Operating pressure, A-2 Over pressure alarm, 4-9 Primary pump head, 2-32 Priming, 3-10, B-31 Priming problems, 4-14 Secondary pump head, 2-33 Selecting the pressure unit, C-16 Setting pressure limits, C-16 Troubleshooting, 4-16 Under pressure alarm, 4-10 Pump check valve leaking, 4-12 Pump components, 2-32 Pump degas See Vacuum degas assembly
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Pump head waste valve Leaking, 4-13 O-ring replacement procedure, 5-23 Pump heads, 5-16 Pump motor lost control alarm, 4-9 Pump page, C-16 Changing the pressure unit, C-16 Setting degas parameters, C-17 Setting pressure limits, C-16 Pump pressure hardware error, 4-9 Pump priming valve O-ring replacement procedure, 5-23 Pump specifications Flow rate, A-2 Operating pressure, A-2 Type, A-2
R Range, C-11, C-26 Rear panel, 2-10 Analog output connector, 2-10 Power receptacle, 2-11 USB connections, 2-10 Rebuilding the injection valve, 5-15 Recorders Analog output setting, C-26 Relay connections AS40, B-111 Rear panel connector, 2-11, D-1 Relay outputs Controlling, D-5 Voltage and current specifications, D-2 Remote Mode, C-10 Reordering information, E-1 Reproducibility, 2-43 Reservoir Connecting, 3-9 Filling, 3-7 Monitoring liquid level in, 3-7, B-30 Restriction in liquid lines, 4-9, 5-10 Retention time Adjusting, F-1
Index-9
ICS-2000 Ion Chromatography System Moving, F-1 Troubleshooting, 4-20 Reverse peaks, C-25 Rise time, C-25 Run time, 2-15 Running samples, 3-18 See also Processing samples
S Safety messages, 1-6 Sample loop, 2-8, 2-40 Changing, 5-14 Injecting, 2-40 Injection valve connections, 2-40, 5-15 Loading, 2-40 Reordering, E-2 Sample processing, 3-2, 3-18 – 3-19 Batch, 3-2, 3-19 Manual, 3-2, 3-18 With Chromeleon, 3-18 – 3-19 Samples Collecting and storing, 3-13 Diluting, 3-14 Filtering, 3-13 Injecting, 3-14, 3-16 Loading, 3-14 Pretreating, 3-13 Saving data, 3-18 – 3-19 Schematics, 2-23 Seal replacement, 5-19 Selectivity Troubleshooting, 4-20 Self-Regenerating Suppressor, 2-9 See also Suppressor Separation process, 1-3 Separator column, 2-8, B-23 Installation, B-24 Sequence, 2-12 Creating, 3-20 Sequence Wizard, 3-20 Serial number, B-19 EluGen cartridge, C-19
Index-10
Server Configuration program AS50 configuration properties, B-21 Starting, 3-4, B-13 Timebase, B-18 Service chase, 2-6, 2-9 Service procedures, 5-17 Check valve cleaning, 5-16 – 5-17 Check valve replacement, 5-16 Conductivity cell replacement, 5-25 CR-TC replacement, 5-60 EGC CO3 Mixer replacement, 5-69 EGC holder replacement, 5-80 Eluent generator cartridge replacement, 5-38 EPM replacement, 5-64 Fuse replacement, 5-37 Injection valve rebuilding, 5-15 Isolation of liquid lines restriction, 5-10 Leak sensor replacement, 5-35 Piston replacement, 5-22 Piston seal replacement, 5-18 Priming valve O-ring replacement, 5-23 Rebuilding the injection valve, 5-15 Replacing tubing and fittings, 5-14 Suppressor replacement, 5-28 Tubing and fittings replacement, 5-14 Waste valve O-ring replacement, 5-23 Sharable device, B-20 Signal plot, 2-16, 2-19 Signal-to-noise ratio, C-25 Sodium hydroxide eluent, 2-35 Software license, B-5 – B-6 Specifications Column heater, A-4 Conductivity cell, A-3 Electrical, A-1 Eluent generator, A-4 Environmental, A-1 Injection valve, A-3 LCD touch screen, A-2 Physical, A-1 Pump, A-2 Vacuum degas assembly, A-3
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Index Stand-alone operation, D-7 – D-11 Analog output connection, D-10 AS/AS50 (USB) setup, D-9, D-11 Example connections, D-8 TTL and relay connections, D-7 Standards When to remake, F-1 – F-2 Starting Chromeleon, B-95 Status page, C-10, C-12 Sulfite in samples, 3-13 Suppression description, 1-3 Suppressor Controlling the current to, 2-19, C-23 Description, 2-9, 2-42 Gas separator waste tube, 2-35 Installation, B-25 Leaking, 4-13 Replacement procedure, 5-28 Selecting the type, C-23 Suppressor alarms Suppressor not connected, 4-11 Suppressor over current, 4-10 Suppressor over power, 4-10 – 4-11 Suppressor stopped for zero flow rate, 4-11 Suppressor page, C-23 Syringe injection, 3-15 Vacuum, 3-16 System Shutdown, 2-16, F-2 Startup, 2-16, 3-3 Status, 3-12 System backpressure, 2-34 System components Descriptions, 2-30 System Control panel, 2-13, 3-5, B-118 See also Control panel System overview, 1-4 System properties dialog box, B-19
T Technical Support, 4-1, 5-1 Temperature
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Cell heater, 2-43, C-9 Column heater, 2-8, 2-42, C-8 Minimizing the effect of variations, 2-43 Temperature compensation, 2-43, A-3 Time, 2-15 Timebase (Chromeleon), 3-5 Adding devices to a timebase, B-20 Assigning the ICS to a timebase, B-15, B-18 Time-out (screen), C-28 TO MODULE USB port connections, B-11 Top cover, 2-6 Total conductivity, C-9, C-28 Touch screen, 2-1, C-1 Adjusting the contrast, 2-2, C-1 Number keypad, 2-3, C-2 Operation, 2-2, C-1 Specifications, A-2 Time-out, C-28 Using with Chromeleon, C-4 Touch screen pages Busy page, C-28 Detector page, C-24 Diagnostic pages, C-30 Eluent Generator page, C-19 Home page, 2-2, C-1, C-6, C-9 – C-10 Information page, C-27 Input/Output page, C-29, D-9 Module Setup page, C-28 Overview, C-5 Plot page, C-10 – C-11 Pump page, C-16 Status page, C-10, C-12 Suppressor page, C-23 Troubleshooting, 4-1 Alarm conditions, 4-3 Baseline noise or drift, 4-22 Calibrations, 5-1 Diagnostics, 5-1 Error messages, 4-3 Excessive backpressure, 4-18 Flow rate, 4-17 High cell output, 4-21
Index-11
ICS-2000 Ion Chromatography System Installation, B-120 Liquid leaks, 4-12 No cell response, 4-20 Peak ghosting, 4-19 Peak height, 4-20 Pump, 4-14 – 4-16 Retention time, 4-20 Selectivity, 4-20 Vacuum degas assembly, 4-23 TTL and relay connector, D-1 Connection instructions, D-2 Pin assignments, D-1 TTL inputs Assigning functions to, D-4, D-9 Control type, D-9 Default function assignments, D-2 Rear panel connector, 2-11 TTL outputs Controlling, D-5 Rear panel connector, 2-11 Tubing Replacing, 5-14 Requirements, 5-14 Routing clips, 2-11 Tubing connections Isolating a restriction, 4-9, 5-10 TUV, 1-8
Specifications, A-3 Troubleshooting, 4-14 Valve See Eluent valve See Injection valve See Waste valve Version number, C-27
W Warranty, voiding, 5-1 Waste container, 5-80 Preventing gas buildup, B-28 Waste lines Blocked, 4-12 Connection, B-27 Connection to AS50, B-109 Gas separator waste tube, 2-35 Waste valve, 2-33 Opening, 2-33, 5-18 O-ring replacement procedure, 5-23 Water samples, 3-13 Weekly maintenance, 3-22 Weight, A-1 Wellness panel, 2-13, 5-1
Y U
Yearly maintenance, 3-22
Unpacking, B-2 Computer, B-4 USB cable, B-11 USB connections, 2-10, B-10 – B-11
Z Zero position (analog out), C-26 Zeroing the baseline, 2-19, C-9
V Vacuum degas assembly, 2-30 Calibration, 5-9 Components, 2-30 Fails to run, 4-23 Setting operating parameters, C-17
Index-12
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